data_exp_288
_audit_creation_date               2021-01-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number       '2016/6'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C15 H21 Co O6'
_chemical_formula_sum              'C15 H21 Co O6'
_chemical_formula_weight           356.25
_chemical_melting_point            ?
_chemical_oxdiff_formula           'Co O6 C15 H21'
_chemical_oxdiff_usercomment       'ST Co(acac)3 rxt from EtOAC by slow evap'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/c 1'
_space_group_name_Hall             '-P 2ybc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'

_cell_length_a                     13.9224(14)
_cell_length_b                     7.4694(7)
_cell_length_c                     16.2302(14)
_cell_angle_alpha                  90
_cell_angle_beta                   98.394(9)
_cell_angle_gamma                  90
_cell_volume                       1669.7(3)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      1895
_cell_measurement_temperature      293(2)
_cell_measurement_theta_max        24.3160
_cell_measurement_theta_min        2.7640
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.052
_exptl_absorpt_correction_T_max    0.989
_exptl_absorpt_correction_T_min    0.955
_exptl_absorpt_correction_type     analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.55a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear dark green'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     dark
_exptl_crystal_colour_primary      green
_exptl_crystal_density_diffrn      1.417
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         needle
_exptl_crystal_F_000               744
loop_
  _exptl_crystal_face_index_h
  _exptl_crystal_face_index_k
  _exptl_crystal_face_index_l
  _exptl_crystal_face_perp_dist
 0 0 -1 0.0709
 0 0 1 0.0708
 0 2 1 0.2793
 0 -2 -1 0.2223
 -1 0 0 0.0270
 1 0 0 0.0400
 1 -1 2 0.1513

_exptl_crystal_size_max            0.535
_exptl_crystal_size_mid            0.153
_exptl_crystal_size_min            0.067
loop_
  _exptl_oxdiff_crystal_face_indexfrac_h
  _exptl_oxdiff_crystal_face_indexfrac_k
  _exptl_oxdiff_crystal_face_indexfrac_l
  _exptl_oxdiff_crystal_face_x
  _exptl_oxdiff_crystal_face_y
  _exptl_oxdiff_crystal_face_z
 -0.0002 -0.0001 -1.0007 0.0302 -0.0311 -0.0086
 0.0002 0.0001 1.0007 -0.0302 0.0311 0.0086
 0.0024 2.0020 0.9996 -0.0546 -0.0407 0.1828
 -0.0024 -2.0020 -0.9996 0.0546 0.0407 -0.1828
 -1.0014 -0.0000 -0.0006 0.0419 0.0254 0.0163
 1.0014 0.0000 0.0006 -0.0419 -0.0254 -0.0163
 1.0006 -1.0007 2.0025 -0.0900 0.0728 -0.0862

_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0340
_diffrn_reflns_av_unetI/netI       0.0522
_diffrn_reflns_Laue_measured_fraction_full  0.954
_diffrn_reflns_Laue_measured_fraction_max  0.915
_diffrn_reflns_limit_h_max         19
_diffrn_reflns_limit_h_min         -12
_diffrn_reflns_limit_k_max         9
_diffrn_reflns_limit_k_min         -10
_diffrn_reflns_limit_l_max         10
_diffrn_reflns_limit_l_min         -22
_diffrn_reflns_number              8932
_diffrn_reflns_point_group_measured_fraction_full  0.954
_diffrn_reflns_point_group_measured_fraction_max  0.915
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           29.128
_diffrn_reflns_theta_min           2.537
_diffrn_ambient_temperature        293(2)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_measured_fraction_theta_full  0.954
_diffrn_measured_fraction_theta_max  0.915
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     29.00  55.00   0.50  120.00    --   20.00  54.00  30.00   52
  2  ω    -67.00  -4.00   0.50  120.00    --   20.00  54.00 150.00  126
  3  ω      5.00  31.00   0.50  120.00    --   20.00  54.00 150.00   52
  4  ω    -71.00 110.00   0.50  120.00    --   20.00  54.00  90.00  362
  5  ω    -73.00 -39.00   0.50  120.00    --   20.00  54.00 -30.00   68
;
_diffrn_measurement_device         'two-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Mini II'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0418254000
_diffrn_orient_matrix_UB_12        -0.0121986000
_diffrn_orient_matrix_UB_13        -0.0301291000
_diffrn_orient_matrix_UB_21        -0.0253403000
_diffrn_orient_matrix_UB_22        -0.0358265000
_diffrn_orient_matrix_UB_23        0.0311319000
_diffrn_orient_matrix_UB_31        -0.0162498000
_diffrn_orient_matrix_UB_32        0.0870516000
_diffrn_orient_matrix_UB_33        0.0085596000
_diffrn_oxdiff_digest_frames
;
017f5f03ea6143ff7c77fc979dd28fda1d006602dad
;
_diffrn_oxdiff_digest_hkl
;
01657a1a66a22553ba8023451908ca65103248
;
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'fine-focus sealed X-ray tube'
_diffrn_source_type                'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  2766
_reflns_number_total               4101
_reflns_odcompleteness_completeness  93.26
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       26.32
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_data_collection         'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_data_reduction          'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.322
_refine_diff_density_min           -0.304
_refine_diff_density_rms           0.064
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     0.996
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       205
_refine_ls_number_reflns           4101
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0801
_refine_ls_R_factor_gt             0.0495
_refine_ls_restrained_S_all        0.996
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0665P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1177
_refine_ls_wR_factor_ref           0.1301
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Co1 Co 0.25810(3) 0.73123(5) 0.53130(2) 0.04396(15) Uani 1 1 d . . . . .
 O1 O 0.24721(14) 0.4982(3) 0.48503(11) 0.0508(5) Uani 1 1 d . . . . .
 O2 O 0.13464(15) 0.8120(3) 0.48109(12) 0.0503(5) Uani 1 1 d . . . . .
 O3 O 0.19847(15) 0.6444(2) 0.62070(11) 0.0520(5) Uani 1 1 d . . . . .
 O4 O 0.28225(14) 0.9647(2) 0.57346(11) 0.0523(5) Uani 1 1 d . . . . .
 O5 O 0.37666(17) 0.6588(3) 0.59239(12) 0.0598(5) Uani 1 1 d . . . . .
 O6 O 0.30868(16) 0.8085(3) 0.43582(11) 0.0529(5) Uani 1 1 d . . . . .
 C1 C 0.1800(3) 0.2500(4) 0.4107(2) 0.0719(10) Uani 1 1 d . . . . .
 H1A H 0.213261 0.251275 0.362897 0.108 Uiso 1 1 calc GR . . . .
 H1B H 0.116419 0.199884 0.395673 0.108 Uiso 1 1 calc GR . . . .
 H1C H 0.216028 0.178837 0.453867 0.108 Uiso 1 1 calc GR . . . .
 C2 C 0.1713(2) 0.4395(4) 0.44190(16) 0.0488(7) Uani 1 1 d . . . . .
 C3 C 0.0850(2) 0.5334(4) 0.42162(19) 0.0589(8) Uani 1 1 d . . . . .
 H3 H 0.032573 0.471895 0.392709 0.071 Uiso 1 1 calc R . . . .
 C4 C 0.0706(2) 0.7112(4) 0.44085(18) 0.0516(7) Uani 1 1 d . . . . .
 C5 C -0.0250(3) 0.7998(5) 0.4116(2) 0.0734(10) Uani 1 1 d . . . . .
 H5A H -0.038126 0.887334 0.451851 0.110 Uiso 1 1 calc GR . . . .
 H5B H -0.075564 0.711319 0.405229 0.110 Uiso 1 1 calc GR . . . .
 H5C H -0.022561 0.857459 0.359111 0.110 Uiso 1 1 calc GR . . . .
 C6 C 0.1441(3) 0.6402(5) 0.75050(19) 0.0712(10) Uani 1 1 d . . . . .
 H6A H 0.080144 0.687808 0.750790 0.107 Uiso 1 1 calc GR . . . .
 H6B H 0.182021 0.657285 0.804264 0.107 Uiso 1 1 calc GR . . . .
 H6C H 0.139787 0.514635 0.737859 0.107 Uiso 1 1 calc GR . . . .
 C7 C 0.1919(2) 0.7355(4) 0.68561(17) 0.0495(7) Uani 1 1 d . . . . .
 C8 C 0.2231(2) 0.9109(4) 0.69993(18) 0.0563(8) Uani 1 1 d . . . . .
 H8 H 0.215792 0.961583 0.750986 0.068 Uiso 1 1 calc R . . . .
 C9 C 0.2642(2) 1.0160(4) 0.64416(16) 0.0471(6) Uani 1 1 d . . . . .
 C10 C 0.2913(3) 1.2071(4) 0.6650(2) 0.0638(9) Uani 1 1 d . . . . .
 H10A H 0.360701 1.218663 0.673923 0.096 Uiso 1 1 calc GR . . . .
 H10B H 0.266057 1.241587 0.714679 0.096 Uiso 1 1 calc GR . . . .
 H10C H 0.264405 1.283247 0.619814 0.096 Uiso 1 1 calc GR . . . .
 C11 C 0.5441(3) 0.6243(6) 0.6303(2) 0.0969(13) Uani 1 1 d . . . . .
 H11A H 0.563098 0.719468 0.669008 0.145 Uiso 1 1 calc GR . . . .
 H11B H 0.597277 0.594681 0.601245 0.145 Uiso 1 1 calc GR . . . .
 H11C H 0.526376 0.521054 0.659903 0.145 Uiso 1 1 calc GR . . . .
 C12 C 0.4582(3) 0.6838(5) 0.5684(2) 0.0662(9) Uani 1 1 d . . . . .
 C13 C 0.4730(3) 0.7586(5) 0.4931(3) 0.0826(12) Uani 1 1 d . . . . .
 H13 H 0.536701 0.773109 0.483371 0.099 Uiso 1 1 calc R . . . .
 C14 C 0.3990(3) 0.8134(5) 0.4311(2) 0.0645(9) Uani 1 1 d . . . . .
 C15 C 0.4212(3) 0.8840(6) 0.3487(2) 0.0952(13) Uani 1 1 d . . . . .
 H15A H 0.408361 0.792370 0.307033 0.143 Uiso 1 1 calc GR . . . .
 H15B H 0.488313 0.918202 0.354093 0.143 Uiso 1 1 calc GR . . . .
 H15C H 0.381068 0.986225 0.332491 0.143 Uiso 1 1 calc GR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Co1 O1 1.893(2) . ?
 Co1 O2 1.890(2) . ?
 Co1 O3 1.8887(17) . ?
 Co1 O4 1.8853(19) . ?
 Co1 O5 1.877(2) . ?
 Co1 O6 1.8838(19) . ?
 O1 C2 1.259(3) . ?
 O2 C4 1.272(4) . ?
 O3 C7 1.269(3) . ?
 O4 C9 1.269(3) . ?
 O5 C12 1.267(4) . ?
 O6 C14 1.272(4) . ?
 C1 H1A 0.9600 . ?
 C1 H1B 0.9600 . ?
 C1 H1C 0.9600 . ?
 C1 C2 1.514(4) . ?
 C2 C3 1.388(4) . ?
 C3 H3 0.9300 . ?
 C3 C4 1.386(4) . ?
 C4 C5 1.501(4) . ?
 C5 H5A 0.9600 . ?
 C5 H5B 0.9600 . ?
 C5 H5C 0.9600 . ?
 C6 H6A 0.9600 . ?
 C6 H6B 0.9600 . ?
 C6 H6C 0.9600 . ?
 C6 C7 1.504(4) . ?
 C7 C8 1.389(4) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.384(4) . ?
 C9 C10 1.502(4) . ?
 C10 H10A 0.9600 . ?
 C10 H10B 0.9600 . ?
 C10 H10C 0.9600 . ?
 C11 H11A 0.9600 . ?
 C11 H11B 0.9600 . ?
 C11 H11C 0.9600 . ?
 C11 C12 1.512(5) . ?
 C12 C13 1.385(5) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.393(5) . ?
 C14 C15 1.511(4) . ?
 C15 H15A 0.9600 . ?
 C15 H15B 0.9600 . ?
 C15 H15C 0.9600 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O2 Co1 O1 96.15(9) . . ?
 O3 Co1 O1 88.28(8) . . ?
 O3 Co1 O2 88.10(9) . . ?
 O4 Co1 O1 173.78(8) . . ?
 O4 Co1 O2 87.94(9) . . ?
 O4 Co1 O3 96.55(8) . . ?
 O5 Co1 O1 87.58(9) . . ?
 O5 Co1 O2 173.69(8) . . ?
 O5 Co1 O3 86.93(9) . . ?
 O5 Co1 O4 88.77(9) . . ?
 O5 Co1 O6 96.74(9) . . ?
 O6 Co1 O1 88.47(8) . . ?
 O6 Co1 O2 88.47(9) . . ?
 O6 Co1 O3 175.00(9) . . ?
 O6 Co1 O4 86.96(8) . . ?
 C2 O1 Co1 123.59(18) . . ?
 C4 O2 Co1 123.88(19) . . ?
 C7 O3 Co1 123.15(19) . . ?
 C9 O4 Co1 124.00(18) . . ?
 C12 O5 Co1 123.6(2) . . ?
 C14 O6 Co1 123.4(2) . . ?
 H1A C1 H1B 109.5 . . ?
 H1A C1 H1C 109.5 . . ?
 H1B C1 H1C 109.5 . . ?
 C2 C1 H1A 109.5 . . ?
 C2 C1 H1B 109.5 . . ?
 C2 C1 H1C 109.5 . . ?
 O1 C2 C1 114.2(3) . . ?
 O1 C2 C3 125.7(3) . . ?
 C3 C2 C1 120.2(3) . . ?
 C2 C3 H3 117.3 . . ?
 C4 C3 C2 125.4(3) . . ?
 C4 C3 H3 117.3 . . ?
 O2 C4 C3 124.7(3) . . ?
 O2 C4 C5 115.1(3) . . ?
 C3 C4 C5 120.2(3) . . ?
 C4 C5 H5A 109.5 . . ?
 C4 C5 H5B 109.5 . . ?
 C4 C5 H5C 109.5 . . ?
 H5A C5 H5B 109.5 . . ?
 H5A C5 H5C 109.5 . . ?
 H5B C5 H5C 109.5 . . ?
 H6A C6 H6B 109.5 . . ?
 H6A C6 H6C 109.5 . . ?
 H6B C6 H6C 109.5 . . ?
 C7 C6 H6A 109.5 . . ?
 C7 C6 H6B 109.5 . . ?
 C7 C6 H6C 109.5 . . ?
 O3 C7 C6 114.9(3) . . ?
 O3 C7 C8 125.9(3) . . ?
 C8 C7 C6 119.3(3) . . ?
 C7 C8 H8 117.5 . . ?
 C9 C8 C7 125.1(3) . . ?
 C9 C8 H8 117.5 . . ?
 O4 C9 C8 125.1(3) . . ?
 O4 C9 C10 114.5(3) . . ?
 C8 C9 C10 120.4(3) . . ?
 C9 C10 H10A 109.5 . . ?
 C9 C10 H10B 109.5 . . ?
 C9 C10 H10C 109.5 . . ?
 H10A C10 H10B 109.5 . . ?
 H10A C10 H10C 109.5 . . ?
 H10B C10 H10C 109.5 . . ?
 H11A C11 H11B 109.5 . . ?
 H11A C11 H11C 109.5 . . ?
 H11B C11 H11C 109.5 . . ?
 C12 C11 H11A 109.5 . . ?
 C12 C11 H11B 109.5 . . ?
 C12 C11 H11C 109.5 . . ?
 O5 C12 C11 114.2(3) . . ?
 O5 C12 C13 125.8(3) . . ?
 C13 C12 C11 120.0(4) . . ?
 C12 C13 H13 117.7 . . ?
 C12 C13 C14 124.5(4) . . ?
 C14 C13 H13 117.7 . . ?
 O6 C14 C13 125.5(3) . . ?
 O6 C14 C15 113.3(3) . . ?
 C13 C14 C15 121.2(3) . . ?
 C14 C15 H15A 109.5 . . ?
 C14 C15 H15B 109.5 . . ?
 C14 C15 H15C 109.5 . . ?
 H15A C15 H15B 109.5 . . ?
 H15A C15 H15C 109.5 . . ?
 H15B C15 H15C 109.5 . . ?


_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  6.412
_oxdiff_exptl_absorpt_empirical_full_min  0.744
