A homochiral magnet based on D3 symmetric [(NaO3)Co3] clusters: from spontaneous resolution to absolute chiral induction
Ru-Xin Yao; Xin Cui; Jun Wang; Xian-Ming Zhang; Chem.Commun. 51 (2015) 5108–; doi:10.1039/C5cc00003C

data_7116732
_publ_section_title
;
 A homochiral magnet based on D3 symmetric [(NaO3)Co3] clusters: from
 spontaneous resolution to absolute chiral induction
;
_journal_name_full               Chem.Commun.
_journal_page_first              5108
_journal_paper_doi               10.1039/C5cc00003C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'0.5(C72 H48 Co6 N24 Na2 O24), N1 O3, 0.25(O1)'
_chemical_formula_sum            'C36 H24 Co3 N13 Na O15.25'
_chemical_formula_weight         1082.46
_chemical_name_systematic        '[NaCo3(IA)6](NO3)'
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-10-31 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.1191(3)
_cell_length_b                   13.1191(3)
_cell_length_c                   16.0140(5)
_cell_measurement_reflns_used    1807
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8500
_cell_measurement_theta_min      3.8820
_cell_volume                     2386.92(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0710
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega    0.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 28

  2 omega  -27.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000    0.0000 30

  3 omega -117.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 82

  4 omega  -41.00   27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -120.0000 68

  5 omega   38.00  105.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892 -111.0000  150.0000 67

  6 omega   43.00   69.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -25.0000    0.0000 26

  7 omega   68.00  102.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -50.0000 -150.0000 34

  8 omega   42.00   93.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -38.0000   90.0000 51

  9 omega   40.00  115.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892 -111.0000 -120.0000 75

 10 omega   38.00   92.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -25.0000   30.0000 54
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1316295000
_diffrn_orient_matrix_UB_12      0.0413873000
_diffrn_orient_matrix_UB_13      0.0118010000
_diffrn_orient_matrix_UB_21      0.0302956000
_diffrn_orient_matrix_UB_22      0.1284624000
_diffrn_orient_matrix_UB_23      -0.0134615000
_diffrn_orient_matrix_UB_31      -0.0120164000
_diffrn_orient_matrix_UB_32      0.0132189000
_diffrn_orient_matrix_UB_33      0.0944538000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.027
_diffrn_reflns_theta_min         2.759
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.025(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         1878
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0706P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                1750
_reflns_number_total             1878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc00003c3.cif
_cod_data_source_block           a
_cod_original_cell_volume        2386.92(13)
_cod_database_code               7116732
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'Co C N O H Na'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: O6(0.08333)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C9(H9), C2(H2), C3(H3), C5(H5), C6(H6), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'