#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:56:23 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180281 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/67/7116732.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7116732
loop_
_publ_author_name
'Ru-Xin Yao'
'Xin Cui'
'Jun Wang'
'Xian-Ming Zhang'
_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       'ω 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/[σ²(Fo²)+(0.0706P)²]
 where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            c5cc00003c3.cif
_cod_data_source_block           a
_cod_original_cell_volume        2386.92(13)
_cod_database_code               7116732
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'Co C N O H Na'
_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.
;
_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'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
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
Co1 Co 0.47336(10) 0.51793(10) 0.27171(11) 0.0243(2) Uani 1 1 d . . .
Na1 Na 0.3333 0.6667 0.2704(4) 0.0229(7) Uani 1 3 d S T P
C7 C 0.5633(7) 0.6918(6) 0.1460(5) 0.0288(16) Uani 1 1 d . . .
O2 O 0.3812(7) 0.3739(6) 0.3752(3) 0.0464(16) Uani 1 1 d . . .
O3 O 0.4749(5) 0.6407(5) 0.1947(3) 0.0307(12) Uani 1 1 d . . .
C8 C 0.5518(9) 0.7663(9) 0.0787(5) 0.043(2) Uani 1 1 d . . .
H8 H 0.4855 0.7747 0.0777 0.052 Uiso 1 1 calc R . .
C1 C 0.3322(7) 0.4317(7) 0.3923(5) 0.0296(17) Uani 1 1 d . . .
O4 O 0.6501(6) 0.6813(7) 0.1509(4) 0.0513(17) Uani 1 1 d . . .
O1 O 0.3410(5) 0.5126(5) 0.3424(4) 0.0352(13) Uani 1 1 d . . .
C11 C 0.5453(9) 0.9026(8) -0.0856(5) 0.042(2) Uani 1 1 d . . .
H11 H 0.4683 0.8697 -0.0665 0.051 Uiso 1 1 calc R . .
C9 C 0.6323(8) 0.8185(8) 0.0225(5) 0.0431(18) Uani 1 1 d . . .
H9 H 0.6993 0.8120 0.0289 0.052 Uiso 1 1 calc R . .
C10 C 0.6319(9) 0.8871(8) -0.0507(5) 0.045(2) Uani 1 1 d . . .
N4 N 0.7275(8) 0.9474(8) -0.0969(5) 0.056(2) Uani 1 1 d . . .
C2 C 0.2686(8) 0.4088(8) 0.4716(5) 0.0365(18) Uani 1 1 d . . .
H2 H 0.2656 0.3501 0.5058 0.044 Uiso 1 1 calc R . .
C3 C 0.2154(7) 0.4654(7) 0.4978(5) 0.0331(18) Uani 1 1 d . . .
H3 H 0.2115 0.5188 0.4615 0.040 Uiso 1 1 calc R . .
C4 C 0.1621(8) 0.4494(8) 0.5802(5) 0.0359(18) Uani 1 1 d . . .
N2 N 0.1833(8) 0.3944(8) 0.6455(4) 0.053(2) Uani 1 1 d . . .
C5 C 0.0880(8) 0.4833(8) 0.6112(5) 0.0376(19) Uani 1 1 d . . .
H5 H 0.0590 0.5242 0.5814 0.045 Uiso 1 1 calc R . .
C6 C 0.1240(9) 0.3985(10) 0.7122(6) 0.051(2) Uani 1 1 d . . .
H6 H 0.1266 0.3698 0.7648 0.062 Uiso 1 1 calc R . .
C12 C 0.7002(9) 0.9977(9) -0.1560(6) 0.047(2) Uani 1 1 d . . .
H12 H 0.7532 1.0457 -0.1966 0.057 Uiso 1 1 calc R . .
N1 N 0.0613(6) 0.4487(7) 0.6933(4) 0.0362(16) Uani 1 1 d . . .
N3 N 0.5909(7) 0.9741(6) -0.1527(5) 0.0369(16) Uani 1 1 d . . .
N5 N 1.0000 1.0000 -0.0634(19) 0.107(8) Uani 1 3 d S T P
O6 O 1.0000 1.0000 0.192(5) 0.23(7) Uani 0.25 3 d S T P
O5 O 1.0968(10) 1.0146(11) -0.0673(14) 0.172(7) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2 Co1 Na1 105.48(19) . .
O2 Co1 C1 29.4(2) . .
O3 Co1 Na1 46.18(18) . .
O3 Co1 O2 150.4(2) . .
O3 Co1 C1 122.5(3) . .
O3 Co1 O1 92.02(19) . .
O3 Co1 N3 110.5(3) . 6_655
C1 Co1 Na1 76.5(2) . .
O1 Co1 Na1 46.02(18) . .
O1 Co1 O2 59.6(2) . .
O1 Co1 C1 30.5(2) . .
N1 Co1 Na1 127.0(2) 5_554 .
N1 Co1 O2 87.5(2) 5_554 .
N1 Co1 O3 103.3(3) 5_554 .
N1 Co1 C1 109.1(3) 5_554 .
N1 Co1 O1 122.9(3) 5_554 .
N1 Co1 N3 119.3(3) 5_554 6_655
N3 Co1 Na1 112.7(2) 6_655 .
N3 Co1 O2 86.6(3) 6_655 .
N3 Co1 C1 93.1(3) 6_655 .
N3 Co1 O1 104.9(3) 6_655 .
Co1 Na1 Co1 119.997(3) 2_665 .
Co1 Na1 Co1 119.994(3) 3_565 2_665
Co1 Na1 Co1 119.997(3) 3_565 .
O3 Na1 Co1 37.75(13) . .
O3 Na1 Co1 133.5(2) . 3_565
O3 Na1 Co1 96.45(15) 2_665 3_565
O3 Na1 Co1 96.45(15) 3_565 .
O3 Na1 Co1 133.5(2) 3_565 2_665
O3 Na1 Co1 96.45(15) . 2_665
O3 Na1 Co1 37.76(13) 3_565 3_565
O3 Na1 Co1 37.76(13) 2_665 2_665
O3 Na1 Co1 133.5(2) 2_665 .
O3 Na1 O3 96.4(2) 2_665 .
O3 Na1 O3 96.4(2) 2_665 3_565
O3 Na1 O3 96.4(2) 3_565 .
O1 Na1 Co1 136.6(2) . 2_665
O1 Na1 Co1 92.80(16) 2_665 .
O1 Na1 Co1 38.32(14) 3_565 3_565
O1 Na1 Co1 136.6(2) 2_665 3_565
O1 Na1 Co1 38.32(14) 2_665 2_665
O1 Na1 Co1 92.80(16) 3_565 2_665
O1 Na1 Co1 38.33(14) . .
O1 Na1 Co1 136.6(2) 3_565 .
O1 Na1 Co1 92.80(16) . 3_565
O1 Na1 O3 75.95(15) . .
O1 Na1 O3 75.95(15) 2_665 2_665
O1 Na1 O3 89.93(17) 3_565 2_665
O1 Na1 O3 170.60(18) 2_665 3_565
O1 Na1 O3 89.93(18) 2_665 .
O1 Na1 O3 170.60(18) . 2_665
O1 Na1 O3 75.95(15) 3_565 3_565
O1 Na1 O3 89.93(18) . 3_565
O1 Na1 O3 170.60(18) 3_565 .
O1 Na1 O1 98.4(2) 3_565 2_665
O1 Na1 O1 98.4(2) 3_565 .
O1 Na1 O1 98.4(2) 2_665 .
O3 C7 C8 114.7(7) . .
O4 C7 O3 123.9(7) . .
O4 C7 C8 121.4(8) . .
C1 O2 Co1 83.1(5) . .
Co1 O3 Na1 96.1(2) . .
C7 O3 Co1 115.9(5) . .
C7 O3 Na1 143.7(5) . .
C9 C8 C7 121.4(9) . .
O2 C1 Co1 67.5(4) . .
O2 C1 O1 120.4(7) . .
O2 C1 C2 118.6(7) . .
O1 C1 Co1 53.9(4) . .
O1 C1 C2 120.9(7) . .
C2 C1 Co1 166.4(6) . .
Co1 O1 Na1 95.7(2) . .
C1 O1 Co1 95.5(5) . .
C1 O1 Na1 168.5(5) . .
N3 C11 C10 108.3(9) . .
C8 C9 C10 128.6(9) . .
C11 C10 C9 131.9(9) . .
N4 C10 C11 107.0(8) . .
N4 C10 C9 121.1(8) . .
C12 N4 C10 106.9(8) . .
C3 C2 C1 124.6(8) . .
C2 C3 C4 123.9(8) . .
N2 C4 C3 123.7(7) . .
C5 C4 C3 131.2(8) . .
C5 C4 N2 105.1(7) . .
C6 N2 C4 108.2(7) . .
C4 C5 N1 110.4(8) . .
N1 C6 N2 110.9(8) . .
N4 C12 N3 113.4(9) . .
C5 N1 Co1 128.6(6) . 6
C6 N1 Co1 126.1(6) . 6
C6 N1 C5 105.3(7) . .
C11 N3 Co1 130.0(7) . 5_564
C12 N3 Co1 125.3(6) . 5_564
C12 N3 C11 104.4(8) . .
O5 N5 O5 119.7(4) 2_765 .
O5 N5 O5 119.7(4) . 3_675
O5 N5 O5 119.7(4) 2_765 3_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Na1 3.2814(8) .
Co1 O2 2.344(6) .
Co1 O3 2.020(5) .
Co1 C1 2.518(8) .
Co1 O1 2.045(6) .
Co1 N1 2.015(7) 5_554
Co1 N3 2.030(7) 6_655
Na1 Co1 3.2814(8) 3_565
Na1 Co1 3.2814(8) 2_665
Na1 O3 2.381(6) .
Na1 O3 2.381(6) 3_565
Na1 O3 2.381(6) 2_665
Na1 O1 2.373(7) 3_565
Na1 O1 2.373(7) .
Na1 O1 2.373(7) 2_665
C7 O3 1.275(10) .
C7 C8 1.512(11) .
C7 O4 1.217(10) .
O2 C1 1.245(10) .
C8 C9 1.292(12) .
C1 O1 1.286(10) .
C1 C2 1.466(11) .
C11 C10 1.371(13) .
C11 N3 1.352(11) .
C9 C10 1.480(11) .
C10 N4 1.323(12) .
N4 C12 1.303(12) .
C2 C3 1.316(11) .
C3 C4 1.458(10) .
C4 N2 1.376(11) .
C4 C5 1.350(12) .
N2 C6 1.338(11) .
C5 N1 1.378(10) .
C6 N1 1.321(11) .
C12 N3 1.308(12) .
N1 Co1 2.015(7) 6
N3 Co1 2.030(7) 5_564
N5 O5 1.187(11) 2_765
N5 O5 1.187(11) 3_675
N5 O5 1.187(11) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
Co1 O2 C1 O1 11.2(8) .
Co1 O2 C1 C2 -166.5(7) .
Co1 C1 O1 Na1 -167(3) .
Co1 C1 C2 C3 65(3) .
C7 C8 C9 C10 175.3(9) .
O2 C1 O1 Co1 -12.8(9) .
O2 C1 O1 Na1 180(2) .
O2 C1 C2 C3 178.5(9) .
O3 C7 C8 C9 -176.6(9) .
C8 C7 O3 Co1 169.3(5) .
C8 C7 O3 Na1 -41.5(12) .
C8 C9 C10 C11 -9.4(18) .
C8 C9 C10 N4 171.5(11) .
C1 C2 C3 C4 -173.9(8) .
O4 C7 O3 Co1 -9.3(10) .
O4 C7 O3 Na1 139.8(8) .
O4 C7 C8 C9 2.1(14) .
O1 C1 C2 C3 0.8(13) .
C11 C10 N4 C12 0.6(11) .
C9 C10 N4 C12 179.9(9) .
C10 C11 N3 Co1 -174.7(6) 5_564
C10 C11 N3 C12 0.4(11) .
C10 N4 C12 N3 -0.4(13) .
N4 C12 N3 Co1 175.4(7) 5_564
N4 C12 N3 C11 0.0(12) .
C2 C1 O1 Co1 164.8(7) .
C2 C1 O1 Na1 -3(3) .
C2 C3 C4 N2 14.8(15) .
C2 C3 C4 C5 -166.7(10) .
C3 C4 N2 C6 177.9(9) .
C3 C4 C5 N1 -179.7(9) .
C4 N2 C6 N1 2.6(14) .
C4 C5 N1 Co1 -179.7(7) 6
C4 C5 N1 C6 2.7(12) .
N2 C4 C5 N1 -1.1(11) .
N2 C6 N1 Co1 179.0(7) 6
N2 C6 N1 C5 -3.2(13) .
C5 C4 N2 C6 -0.9(12) .
N3 C11 C10 C9 -179.8(9) .
N3 C11 C10 N4 -0.6(11) .
