#------------------------------------------------------------------------------
#$Date: 2019-11-24 00:47:10 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235834 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349788.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_4349788
loop_
_publ_author_name
'Yao, Ru-Xin'
'Fu, Huan-Huan'
'Yu, Bo'
'Zhang, Xian-Ming'
_publ_section_title
;
 Chiral metal--organic frameworks constructed from four-fold helical chain
 SBUs for enantioselective recognition of α-hydroxy/amino acids
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              153
_journal_paper_doi               10.1039/C7QI00615B
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         '0.13(C68 H24 Co8 O40)'
_chemical_formula_sum            'C8.5 H3 Co O5'
_chemical_formula_weight         244.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.33411(15)
_cell_length_b                   15.33411(15)
_cell_length_c                   12.21062(17)
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7070
_cell_measurement_theta_min      4.1920
_cell_volume                     2871.14(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  40.00   1.00   33.27    --   22.24 -38.00-150.00   44
  2  ω     46.00  72.00   1.00   33.27    --   22.24  57.00   0.00   26
  3  ω     -8.00  76.00   1.00   33.27    --   22.24  77.00  90.00   84
  4  ω      7.00  62.00   1.00   33.27    --   22.24 -99.00-150.00   55
  5  ω      7.00  64.00   1.00   33.27    --   22.24 -99.00 -30.00   57
  6  ω    -51.00  94.00   1.00   33.27    --   22.24   0.00 -90.00  145
  7  ω    -99.00 -74.00   1.00   33.27    --  -22.55 178.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0364265000
_diffrn_orient_matrix_UB_12      -0.0255127000
_diffrn_orient_matrix_UB_13      0.0160206000
_diffrn_orient_matrix_UB_21      -0.0278496000
_diffrn_orient_matrix_UB_22      -0.0362474000
_diffrn_orient_matrix_UB_23      0.0088348000
_diffrn_orient_matrix_UB_31      0.0061092000
_diffrn_orient_matrix_UB_32      -0.0132187000
_diffrn_orient_matrix_UB_33      -0.0551322000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13428
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         3.407
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         0.822
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 725 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.220(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0468
_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)+(0.1058P)²+25.0394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1771
_reflns_number_total             1801
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00615b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2871.14(7)
_cod_original_formula_sum        'C8.50 H3 Co O5'
_cod_database_code               4349788
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Co C H O N'
_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.
;
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.732
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O3)
3. Others
 Fixed Sof: C6(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_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 1.106
_oxdiff_exptl_absorpt_empirical_full_min 0.954
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/4'
'x, -y+1/2, -z+1/4'
'-x+1/2, -y+1/2, z+1/2'
'-y, -x, -z'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x, z+3/4'
'-x+1/2, y, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'x+1/2, -y+1, -z+3/4'
'-x+1, -y+1, z+1'
'-y+1/2, -x+1/2, -z+1/2'
'y+1, x+1, -z+1'
'y+1, -x+1/2, z+5/4'
'-x+1, y+1/2, -z+5/4'
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 0.81234(4) 0.31234(4) 0.2500 0.0108(2) Uani 1 2 d S T P
O1 O 0.7114(3) 0.4038(3) 0.2483(4) 0.0334(8) Uani 1 1 d . . .
C4 C 0.5000 0.5000 0.0615(5) 0.0237(14) Uani 1 2 d S T P
C1 C 0.5000 0.5000 0.2897(5) 0.0233(13) Uani 1 2 d S T P
H1 H 0.5000 0.5000 0.3659 0.028 Uiso 1 2 calc RS T P
C2 C 0.5666(4) 0.4607(3) 0.2347(4) 0.0234(12) Uani 1 1 d . . .
C3 C 0.5676(4) 0.4628(3) 0.1185(4) 0.0246(12) Uani 1 1 d . . .
H3 H 0.6145 0.4387 0.0807 0.030 Uiso 1 1 calc R . .
C5 C 0.6384(3) 0.4116(3) 0.2933(4) 0.0196(10) Uani 1 1 d . . .
O2 O 0.6189(3) 0.3813(3) 0.3856(3) 0.0283(8) Uani 1 1 d . . .
O3 O 0.7352(4) 0.2500 0.1250 0.0334(8) Uani 1 2 d S T P
C6 C 0.6585(13) 0.2500 0.1250 0.048(6) Uani 0.5 2 d S T P
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'
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
O1 Co1 O1 174.3(3) 6_545 .
O1 Co1 O3 83.33(16) . .
O1 Co1 O3 92.67(17) 6_545 .
O1 Co1 O3 92.67(17) . 2_645
O1 Co1 O3 83.33(16) 6_545 2_645
O2 Co1 O1 92.4(2) 7_564 6_545
O2 Co1 O1 91.7(2) 7_564 .
O2 Co1 O1 92.4(2) 8_655 .
O2 Co1 O1 91.7(2) 8_655 6_545
O2 Co1 O2 86.2(2) 8_655 7_564
O2 Co1 O3 91.63(13) 8_655 2_645
O2 Co1 O3 175.16(17) 7_564 2_645
O2 Co1 O3 175.16(17) 8_655 .
O2 Co1 O3 91.63(13) 7_564 .
O3 Co1 O3 90.85(14) . 2_645
C5 O1 Co1 136.2(4) . .
C3 C4 C4 120.4(3) 12_554 5_665
C3 C4 C4 120.4(3) . 5_665
C3 C4 C3 119.1(6) . 12_554
C2 C1 C2 120.9(6) . 12_554
C1 C2 C3 119.5(5) . .
C1 C2 C5 122.1(5) . .
C3 C2 C5 118.4(4) . .
C4 C3 C2 120.5(5) . .
O1 C5 C2 119.3(5) . .
O1 C5 O2 124.8(5) . .
O2 C5 C2 115.8(4) . .
C5 O2 Co1 133.0(3) . 2_645
Co1 O3 Co1 113.4(3) 3 .
C6 O3 Co1 123.28(13) . 3
C6 O3 Co1 123.29(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.089(4) .
Co1 O1 2.089(4) 6_545
Co1 O2 2.044(3) 7_564
Co1 O2 2.044(3) 8_655
Co1 O3 2.154(3) 2_645
Co1 O3 2.154(3) .
O1 C5 1.252(6) .
C4 C4 1.502(12) 5_665
C4 C3 1.373(6) .
C4 C3 1.373(6) 12_554
C1 C2 1.363(6) .
C1 C2 1.363(6) 12_554
C2 C3 1.419(7) .
C2 C5 1.514(6) .
C5 O2 1.255(6) .
O2 Co1 2.044(3) 2_645
O3 Co1 2.154(3) 3
O3 C6 1.18(2) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.250 -0.019 686 167 ' '
2 0.750 0.750 -0.018 686 167 ' '
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.250 0.250 -0.035 707.0 124.3
2 -0.250 0.750 -0.433 707.0 124.3
