data_exp_311
_audit_creation_date               2020-11-03
_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           'C6 H24 Co1 N6, 3.5(Cl), 0.5(H12 Na1 O6)'
_chemical_formula_sum              'C6 H30 Cl3.50 Co N6 Na0.50 O3'
_chemical_formula_weight           428.86
_chemical_melting_point            ?
_chemical_oxdiff_formula           'Co2 C12 N12 O2 Cl4 Na'
_chemical_oxdiff_usercomment       'LC prep from chem 110 racemic Co(en)3'
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'
 'Cl' 'Cl' 0.1484 0.1585 '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'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na' 'Na' 0.0362 0.0249 '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        'trigonal'
_space_group_IT_number             165
_space_group_name_H-M_alt          'P -3 c 1'
_space_group_name_Hall             '-P 3 2"c'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z+1/2'
 'x-y, -y, -z+1/2'
 '-x, -x+y, -z+1/2'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z-1/2'
 '-x+y, y, z-1/2'
 'x, x-y, z-1/2'

_cell_length_a                     11.4290(2)
_cell_length_b                     11.4290(2)
_cell_length_c                     15.5815(2)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  120
_cell_volume                       1762.61(7)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      25434
_cell_measurement_temperature      293(2)
_cell_measurement_theta_max        30.5920
_cell_measurement_theta_min        2.0520
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.530
_exptl_absorpt_correction_T_max    0.750
_exptl_absorpt_correction_T_min    0.600
_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 light orange'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      orange
_exptl_crystal_density_diffrn      1.616
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               896
loop_
  _exptl_crystal_face_index_h
  _exptl_crystal_face_index_k
  _exptl_crystal_face_index_l
  _exptl_crystal_face_perp_dist
 -3 -1 5 0.0831
 -2 5 0 0.2152
 2 -5 0 0.1260
 -5 0 -3 0.1574
 5 0 3 0.0883
 0 0 -1 0.1083
 0 0 1 0.1083
 0 1 -1 0.1341
 3 -5 -5 0.1159
 -5 5 -3 0.1820
 -1 1 -1 0.1528
 4 1 5 0.0771
 -2 0 -5 0.1171

_exptl_crystal_size_max            0.385
_exptl_crystal_size_mid            0.289
_exptl_crystal_size_min            0.217
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
 -2.9987 -0.9967 4.9921 0.0286 -0.2746 0.2050
 -1.9963 4.9937 -0.0001 0.0048 -0.1138 -0.2904
 1.9963 -4.9937 0.0001 -0.0048 0.1138 0.2904
 -4.9921 -0.0042 -2.9965 0.3558 -0.1078 0.0923
 4.9921 0.0042 2.9965 -0.3558 0.1078 -0.0923
 0.0005 -0.0007 -0.9985 0.0302 0.0318 -0.0120
 -0.0005 0.0007 0.9985 -0.0302 -0.0318 0.0120
 0.0007 0.9982 -0.9985 0.0099 0.0253 -0.0803
 2.9974 -4.9968 -4.9925 0.0930 0.3137 0.2050
 -4.9910 4.9903 -2.9962 0.2545 -0.1403 -0.2493
 -0.9980 0.9978 -0.9987 0.0630 -0.0153 -0.0547
 3.9926 1.0041 4.9934 -0.3833 -0.0031 -0.1111
 -1.9950 -0.0043 -4.9930 0.2569 0.0779 -0.0085

_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0274
_diffrn_reflns_av_unetI/netI       0.0086
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.995
_diffrn_reflns_limit_h_max         16
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         16
_diffrn_reflns_limit_k_min         -16
_diffrn_reflns_limit_l_max         22
_diffrn_reflns_limit_l_min         -22
_diffrn_reflns_number              65362
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.995
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           30.885
_diffrn_reflns_theta_min           2.614
_diffrn_ambient_temperature        293(2)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00-150.00  368
  2  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00 -90.00  368
  3  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00 120.00  368
  4  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00-120.00  368
  5  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00-180.00  368
  6  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00 -30.00  368
  7  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00  90.00  368
  8  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00   0.00  368
  9  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00 150.00  368
 10  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00 -60.00  368
 11  ω    -74.00 104.00   0.50   35.00    --   20.00  54.00  60.00  356
 12  ω    -74.00 110.00   0.50   35.00    --   20.00  54.00  30.00  368
;
_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        -0.0531169000
_diffrn_orient_matrix_UB_12        -0.0202769000
_diffrn_orient_matrix_UB_13        -0.0302196000
_diffrn_orient_matrix_UB_21        0.0407150000
_diffrn_orient_matrix_UB_22        -0.0065221000
_diffrn_orient_matrix_UB_23        -0.0318577000
_diffrn_orient_matrix_UB_31        -0.0256482000
_diffrn_orient_matrix_UB_32        -0.0684074000
_diffrn_orient_matrix_UB_33        0.0120073000
_diffrn_oxdiff_digest_frames
;
01db534ee68106cf18685d16e01f877eab04404b4f6
;
_diffrn_oxdiff_digest_hkl
;
01468712754b2bc78c562b7e6f0e9272bc4c5e
;
_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                  1643
_reflns_number_total               1860
_reflns_odcompleteness_completeness  99.95
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       30.44
_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           0.478
_refine_diff_density_min           -0.782
_refine_diff_density_rms           0.062
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.057
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       99
_refine_ls_number_reflns           1860
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0312
_refine_ls_R_factor_gt             0.0267
_refine_ls_restrained_S_all        1.057
_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)+(0.0392P)²+0.8846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0716
_refine_ls_wR_factor_ref           0.0736
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2.a Rotating group:
 O1(H1E)
;
_atom_sites_solution_hydrogens     difmap
_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 0.333333 0.666667 0.88150(2) 0.01757(9) Uani 1 3 d S T P . .
 Cl1 Cl -0.10243(4) 0.51023(4) 0.87483(2) 0.03423(11) Uani 1 1 d . . . . .
 Cl2 Cl 0.000000 0.000000 1.000000 0.0546(3) Uani 1 6 d S T P . .
 Na1 Na 0.000000 0.000000 0.750000 0.0542(5) Uani 1 6 d S T P . .
 N1 N 0.29981(13) 0.51117(12) 0.95318(8) 0.0244(2) Uani 1 1 d . . . . .
 N2 N 0.18594(13) 0.53381(13) 0.80955(8) 0.0273(2) Uani 1 1 d . . . . .
 O1 O 0.19929(18) 0.11081(17) 0.84376(12) 0.0594(4) Uani 1 1 d . . . . .
 H1E H 0.174028 0.099220 0.896198 0.089 Uiso 1 1 d GR . . . .
 C1 C 0.17222(16) 0.39079(15) 0.92573(10) 0.0302(3) Uani 1 1 d . . . . .
 C2 C 0.16420(17) 0.39744(16) 0.82966(10) 0.0316(3) Uani 1 1 d . . . . .
 H2C H 0.235(2) 0.386(2) 0.8001(13) 0.036(5) Uiso 1 1 d . . . . .
 H1A H 0.363(2) 0.494(2) 0.9450(13) 0.037(5) Uiso 1 1 d . . . . .
 H1C H 0.172(2) 0.312(2) 0.9466(15) 0.043(6) Uiso 1 1 d . . . . .
 H1D H 0.104(2) 0.395(2) 0.9506(13) 0.033(5) Uiso 1 1 d . . . . .
 H2D H 0.080(2) 0.332(2) 0.8100(13) 0.040(5) Uiso 1 1 d . . . . .
 H2A H 0.114(2) 0.533(2) 0.8201(13) 0.037(5) Uiso 1 1 d . . . . .
 H1B H 0.291(2) 0.519(2) 1.0036(15) 0.040(6) Uiso 1 1 d . . . . .
 H2B H 0.198(2) 0.547(2) 0.7572(14) 0.041(6) Uiso 1 1 d . . . . .
 H1F H 0.282(4) 0.180(4) 0.852(2) 0.092(11) Uiso 1 1 d . . . . .


_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 N1 1.9677(12) 3_565 ?
 Co1 N1 1.9677(12) 2_665 ?
 Co1 N1 1.9677(12) . ?
 Co1 N2 1.9601(12) 3_565 ?
 Co1 N2 1.9601(12) 2_665 ?
 Co1 N2 1.9602(12) . ?
 Na1 O1 2.4579(19) 4_556 ?
 Na1 O1 2.4579(19) . ?
 Na1 O1 2.4579(19) 6_556 ?
 Na1 O1 2.4579(19) 5_556 ?
 Na1 O1 2.4579(19) 3 ?
 Na1 O1 2.4579(19) 2 ?
 N1 C1 1.4819(19) . ?
 N1 H1A 0.84(2) . ?
 N1 H1B 0.80(2) . ?
 N2 C2 1.484(2) . ?
 N2 H2A 0.83(2) . ?
 N2 H2B 0.83(2) . ?
 O1 H1E 0.8546 . ?
 O1 H1F 0.88(4) . ?
 C1 C2 1.504(2) . ?
 C1 H1C 0.95(2) . ?
 C1 H1D 0.90(2) . ?
 C2 H2C 1.00(2) . ?
 C2 H2D 0.93(2) . ?

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
 N1 Co1 N1 90.95(5) 3_565 2_665 ?
 N1 Co1 N1 90.95(5) 3_565 . ?
 N1 Co1 N1 90.95(5) 2_665 . ?
 N2 Co1 N1 174.50(5) 3_565 . ?
 N2 Co1 N1 174.50(6) 2_665 3_565 ?
 N2 Co1 N1 85.48(5) 2_665 2_665 ?
 N2 Co1 N1 85.48(5) . . ?
 N2 Co1 N1 85.48(5) 3_565 3_565 ?
 N2 Co1 N1 93.29(6) 2_665 . ?
 N2 Co1 N1 93.29(6) . 3_565 ?
 N2 Co1 N1 174.50(5) . 2_665 ?
 N2 Co1 N1 93.29(6) 3_565 2_665 ?
 N2 Co1 N2 90.53(6) 3_565 2_665 ?
 N2 Co1 N2 90.54(6) 3_565 . ?
 N2 Co1 N2 90.54(6) . 2_665 ?
 O1 Na1 O1 88.29(6) 2 . ?
 O1 Na1 O1 174.05(8) 6_556 . ?
 O1 Na1 O1 88.29(6) 6_556 5_556 ?
 O1 Na1 O1 88.29(6) 5_556 4_556 ?
 O1 Na1 O1 174.04(8) 5_556 2 ?
 O1 Na1 O1 87.73(9) 4_556 . ?
 O1 Na1 O1 88.29(6) 2 3 ?
 O1 Na1 O1 174.04(8) 4_556 3 ?
 O1 Na1 O1 96.02(8) 5_556 . ?
 O1 Na1 O1 96.02(8) 2 4_556 ?
 O1 Na1 O1 88.29(6) 3 . ?
 O1 Na1 O1 96.02(8) 6_556 3 ?
 O1 Na1 O1 87.73(9) 5_556 3 ?
 O1 Na1 O1 87.73(9) 6_556 2 ?
 O1 Na1 O1 88.29(6) 6_556 4_556 ?
 Co1 N1 H1A 108.6(14) . . ?
 Co1 N1 H1B 115.5(16) . . ?
 C1 N1 Co1 109.36(9) . . ?
 C1 N1 H1A 107.3(14) . . ?
 C1 N1 H1B 105.6(16) . . ?
 H1A N1 H1B 110(2) . . ?
 Co1 N2 H2A 110.7(15) . . ?
 Co1 N2 H2B 115.1(15) . . ?
 C2 N2 Co1 108.70(9) . . ?
 C2 N2 H2A 107.7(16) . . ?
 C2 N2 H2B 108.7(15) . . ?
 H2A N2 H2B 106(2) . . ?
 Na1 O1 H1E 109.5 . . ?
 Na1 O1 H1F 148(2) . . ?
 H1E O1 H1F 96.9 . . ?
 N1 C1 C2 107.27(12) . . ?
 N1 C1 H1C 108.3(14) . . ?
 N1 C1 H1D 107.6(13) . . ?
 C2 C1 H1C 114.5(14) . . ?
 C2 C1 H1D 110.4(13) . . ?
 H1C C1 H1D 108.5(19) . . ?
 N2 C2 C1 106.31(12) . . ?
 N2 C2 H2C 108.8(13) . . ?
 N2 C2 H2D 110.2(13) . . ?
 C1 C2 H2C 112.2(12) . . ?
 C1 C2 H2D 110.7(13) . . ?
 H2C C2 H2D 108.6(18) . . ?


_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  1.129
_oxdiff_exptl_absorpt_empirical_full_min  0.872
