Co(II) coordination polymers constructed from a bent chiral linker: influencing framework topology using co-ligands
Tay, Hui Min; Hua, Carol; CrystEngComm  (2020) –; doi:10.1039/D0CE01172J

data_7241251
_publ_section_title
;
 Co(II) coordination polymers constructed from a bent chiral linker:
 influencing framework topology using co-ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01172J
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C72 H56 Co2 N11.962 O12 S4.038'
_chemical_formula_sum            'C72 H56 Co2 N11.96 O12 S4.04'
_chemical_formula_weight         1528.11
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-08-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-08-10 deposited with the CCDC.	2020-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                73.885(2)
_cell_angle_beta                 80.363(2)
_cell_angle_gamma                84.052(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9800(3)
_cell_length_b                   12.1273(3)
_cell_length_c                   15.6920(4)
_cell_measurement_reflns_used    17601
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.7600
_cell_measurement_theta_min      3.7910
_cell_volume                     1975.47(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(2)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     26.00  52.00   0.50    0.95    --   47.80  77.00   0.00   52
  2  \w     37.00  71.00   0.50    0.95    --   58.00  75.00 -19.04   68
  3  \w     93.00 127.00   0.50    0.95    --   58.00  75.00 -19.04   68
  4  \w    103.00 130.00   0.50    0.95    --   58.00  74.00 -76.58   54
  5  \w     90.00 137.00   0.50    2.50    --  105.64 140.00-118.00   94
  6  \w     80.00 121.00   0.50    0.95    --   50.00  79.00-142.46   82
  7  \w     88.00 174.00   0.50    2.50    --  105.64  77.00-150.00  172
  8  \w    143.00 178.00   0.50    2.50    --  105.64  45.00-180.00   70
  9  \w    152.00 178.00   0.50    2.50    --  105.64  61.00-180.00   52
 10  \w    142.00 178.00   0.50    2.50    --  105.64  77.00 -30.00   72
 11  \w    142.00 169.00   0.50    2.50    --  105.64  61.00  30.00   54
 12  \w    122.00 174.00   0.50    2.50    --  105.64  61.00  90.00  104
 13  \w    104.00 151.00   0.50    2.50    --  105.64  30.00  30.00   94
 14  \w    100.00 175.00   0.50    2.50    --  105.64  45.00  60.00  150
 15  \w     93.00 145.00   0.50    2.50    --  105.64 130.00  68.00  104
 16  \w     93.00 119.00   0.50    2.50    --  105.64  61.00  90.00   52
 17  \w     91.00 173.00   0.50    2.50    --  105.64  61.00 120.00  164
 18  \w     92.00 139.00   0.50    2.50    --  105.64  61.00  30.00   94
 19  \w     85.00 137.00   0.50    2.50    --  105.64  77.00 -30.00  104
 20  \w     97.00 151.00   0.50    2.50    --  105.64  45.00 -90.00  108
 21  \w     95.00 135.00   0.50    2.50    --  105.64  45.00-180.00   80
 22  \w     91.00 132.00   0.50    2.50    --  105.64  61.00-180.00   82
 23  \w     91.00 178.00   0.50    2.50    --  105.64  61.00 -90.00  174
 24  \w     92.00 178.00   0.50    2.50    --  105.64  61.00 -60.00  172
 25  \w     66.00 107.00   0.50    2.50    --   90.00-101.00 -10.33   82
 26  \w     76.00 110.00   0.50    2.50    --  105.64-130.00  -4.00   68
 27  \w     44.00  69.00   0.50    2.50    --  105.64 -61.00-120.00   50
 28  \w     59.00  94.00   0.50    2.50    --  105.64 -77.00-180.00   70
 29  \w     79.00 105.00   0.50    2.50    --  105.64 -94.00-150.00   52
 30  \w     94.00 123.00   0.50    2.50    --  105.64-140.00-177.00   58
 31  \w     45.00  79.00   0.50    0.95    --   47.80-140.00-177.00   68
 32  \w     34.00  96.00   0.50    2.50    --  105.64 -94.00 -60.00  124
 33  \w     41.00 104.00   0.50    2.50    --  105.64 -94.00   0.00  126
 34  \w     38.00  72.00   0.50    0.95    --   47.80-130.00  -4.00   68
 35  \w     34.00 105.00   0.50    2.50    --  105.64 -94.00  90.00  142
 36  \w     65.00 111.00   0.50    2.50    --  105.64-125.00 150.00   92
 37  \w     41.00  71.00   0.50    2.50    --  105.64 -61.00 150.00   60
 38  \w     46.00  71.00   0.50    2.50    --  105.64 -61.00  60.00   50
 39  \w     35.00 101.00   0.50    2.50    --  105.64 -77.00   0.00  132
 40  \w     38.00  74.00   0.50    0.95    --   47.80  19.00 -90.00   72
 41  \w     33.00  60.00   0.50    0.95    --   54.00  76.00 -99.77   54
 42  \w     42.00  76.00   0.50    0.95    --   62.00  76.00 -62.16   68
 43  \w     53.00  78.00   0.50    0.95    --   74.00  77.00 -96.72   50
 44  \w     42.00  97.00   0.50    0.95    --   47.80  19.00-180.00  110
 45  \w     42.00  68.00   0.50    0.95    --   62.00  74.00-148.55   52
 46  \w     37.00  73.00   0.50    0.95    --   58.00  76.00-178.28   72
 47  \w     44.00  70.00   0.50    0.95    --   66.00  77.00-131.64   52
 48  \w     28.00  54.00   0.50    0.95    --   50.00  79.00-142.46   52
 49  \w     29.00  55.00   0.50    0.95    --   50.00  76.00-178.23   52
 50  \w      0.00  25.00   0.50    0.95    --   30.00  95.00-124.62   50
 51  \w     -4.00  21.00   0.50    0.95    --   26.00  95.00 -74.44   50
 52  \w     10.00  36.00   0.50    0.95    --   38.00  91.00 -80.84   52
 53  \w     38.00  65.00   0.50    0.95    --   58.00  74.00 -76.58   54
 54  \w     39.00  64.00   0.50    0.95    --   58.00  73.00  10.99   50
 55  \w     49.00  75.00   0.50    0.95    --   70.00  76.00  11.58   52
 56  \w     44.00  70.00   0.50    0.95    --   66.00  77.00  38.16   52
 57  \w     48.00  74.00   0.50    0.95    --   70.00  77.00  85.77   52
 58  \w     49.00  74.00   0.50    0.95    --   70.00  77.00 157.87   50
 59  \w     26.00  52.00   0.50    0.95    --   47.80  77.00 150.00   52
 60  \w     28.00  98.00   0.50    0.95    --   50.00  78.00  89.90  140
 61  \w     28.00  55.00   0.50    0.95    --   50.00  77.00  50.42   54
 62  \w      9.00  34.00   0.50    0.95    --   38.00  92.00  67.31   50
 63  \w    -39.00 -14.00   0.50    0.95    --    6.00 123.00-100.27   50
 64  \w    -20.00   5.00   0.50    0.95    --   14.00 103.00-161.95   50
 65  \w    -63.00 -37.00   0.50    0.95    --  -47.80 140.00-118.00   52
 66  \w    -59.00 -34.00   0.50    2.50    --  -86.25 140.00-118.00   50
 67  \w    -95.00 -65.00   0.50    0.95    --  -47.80 140.00-118.00   60
 68  \w    -95.00 -69.00   0.50    2.50    --  -86.25 140.00-118.00   52
 69  \w    -84.00 -45.00   0.50    0.95    --  -47.80 130.00  68.00   78
 70  \w    -77.00 -52.00   0.50    2.50    --  -86.25 130.00  68.00   50
 71  \w    -78.00 -38.00   0.50    0.95    --  -47.80 -24.00  91.03   80
 72  \w    -69.00 -28.00   0.50    0.95    --  -47.80 -77.00  60.00   82
 73  \w    -66.00 -41.00   0.50    0.95    --  -62.00 -74.00  87.53   50
 74  \w    -78.00 -51.00   0.50    0.95    --  -66.00 -65.00  68.11   54
 75  \w    -74.00 -49.00   0.50    0.95    --  -66.00 -67.00 113.55   50
 76  \w    -80.00 -47.00   0.50    0.95    --  -66.00 -69.00 138.40   66
 77  \w    -82.00 -55.00   0.50    2.50    --  -74.00 -71.00 160.89   54
 78  \w    -84.00 -58.00   0.50    2.50    --  -78.00 -73.00 102.80   52
 79  \w    -73.00 -48.00   0.50    0.95    --  -66.00 -67.00  48.07   50
 80  \w    -69.00 -43.00   0.50    0.95    --  -66.00 -79.00 -36.98   52
 81  \w    -57.00 -32.00   0.50    0.95    --  -54.00 -77.00 -82.90   50
 82  \w    -82.00 -55.00   0.50    2.50    --  -74.00 -71.00  21.82   54
 83  \w    -90.00 -55.00   0.50    2.50    --  -74.00 -71.00 -55.84   70
 84  \w    -92.00 -65.00   0.50    2.50    --  -86.00 -74.00  -1.03   54
 85  \w    -93.00 -66.00   0.50    2.50    --  -86.25 -73.00 -60.60   54
 86  \w    -92.00 -67.00   0.50    2.50    --  -86.25 -70.00 -81.28   50
 87  \w    -91.00 -64.00   0.50    2.50    --  -86.25 -77.00-120.00   54
 88  \w    -84.00 -58.00   0.50    2.50    --  -78.00 -72.00-175.43   52
 89  \w    -92.00 -63.00   0.50    2.50    --  -82.00 -69.00-150.59   58
 90  \w    -88.00 -63.00   0.50    2.50    --  -86.25 -80.00-165.12   50
 91  \w    -93.00 -68.00   0.50    2.50    --  -86.25 -69.00-168.96   50
 92  \w    -92.00 -66.00   0.50    2.50    --  -86.25 -72.00-113.94   52
 93  \w    -94.00 -68.00   0.50    2.50    --  -86.25 -69.00 -89.89   52
 94  \w    -90.00 -65.00   0.50    2.50    --  -86.25 -76.00 -48.29   50
 95  \w   -101.00 -69.00   0.50    2.50    --  -86.25 -71.00  32.00   64
 96  \w   -100.00 -67.00   0.50    2.50    --  -86.25 -71.00 -25.92   66
 97  \w    -93.00 -66.00   0.50    2.50    --  -86.25 -72.00  16.40   54
 98  \w    -89.00 -64.00   0.50    2.50    --  -86.25 -77.00  60.00   50
 99  \w    -86.00 -59.00   0.50    2.50    --  -78.00 -73.00 119.10   54
100  \w    -92.00 -67.00   0.50    2.50    --  -86.25 -71.00  96.11   50
101  \w    -95.00 -64.00   0.50    2.50    --  -86.25 -77.00 150.00   62
102  \w    -92.00 -67.00   0.50    2.50    --  -86.25 -77.00  90.00   50
103  \w    -94.00 -64.00   0.50    2.50    --  -86.25 -78.00  55.39   60
104  \w    -96.00 -71.00   0.50    2.50    --  -86.25 -62.00 119.99   50
105  \w   -112.00 -82.00   0.50    0.95    --  -47.80 -24.00  91.03   60
106  \w   -108.00 -67.00   0.50    2.50    --  -86.25 -72.00 165.50   82
107  \w   -125.00 -68.00   0.50    2.50    --  -86.25 -77.00  81.13  114
108  \w   -119.00 -71.00   0.50    0.95    --  -47.80-130.00  -4.00   96
109  \w     34.00  59.00   0.50    2.50    --  105.64 -61.00-150.00   50
110  \w     35.00  62.00   0.50    2.50    --  105.64 -77.00-120.00   54
111  \w     35.00 105.00   0.50    2.50    --  105.64 -94.00-180.00  140
112  \w   -113.00 -88.00   0.50    0.95    --  -47.80-140.00-177.00   50
113  \w   -134.00-109.00   0.50    2.50    --  -86.25-140.00-177.00   50
114  \w   -146.00-120.00   0.50    2.50    --  -86.25 -80.00-165.12   52
115  \w   -147.00-122.00   0.50    2.50    --  -82.00 -69.00-150.59   50
116  \w   -143.00-110.00   0.50    2.50    --  -86.25 -77.00-120.00   66
117  \w   -110.00 -85.00   0.50    0.95    --  -54.00 -77.00 -82.90   50
118  \w   -125.00-100.00   0.50    2.50    --  -86.25-130.00  -4.00   50
119  \w   -149.00-105.00   0.50    2.50    --  -86.00 -74.00  -1.03   88
120  \w   -152.00-126.00   0.50    2.50    --  -86.25 -70.00 -81.28   52
121  \w   -143.00-107.00   0.50    2.50    --  -86.25 -72.00-113.94   72
122  \w   -155.00-128.00   0.50    2.50    --  -86.25 -69.00-168.96   54
123  \w   -157.00-132.00   0.50    2.50    --  -86.25 -73.00 -60.60   50
124  \w   -146.00-116.00   0.50    2.50    --  -86.25 -71.00  32.00   60
125  \w   -158.00-121.00   0.50    2.50    --  -86.25 -77.00  90.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52448
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.241
_diffrn_reflns_theta_min         2.963
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       plate
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.960
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.033(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         14922
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1486P)^2^+4.4938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2544
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                12622
_reflns_number_total             14922
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 70.0678\% 
 around [0.68 -0.45 -0.58] (reciprocal) or [0.87 -0.37 -0.33] (direct)
;
_cod_data_source_file            d0ce01172j2.cif
_cod_data_source_block           compound_4
_cod_database_code               7241251
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.326
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.967(7)
 0.033(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C50) = Uanis(C51) = Uanis(C49) = Uanis(C16) = Uanis(C18) = Uanis(C17)
4. Others
 Sof(N9)=1-FVAR(1)
 Sof(S009)=FVAR(1)
 Sof(N6)=1-FVAR(2)
 Sof(S007)=FVAR(2)
 Sof(N7)=1-FVAR(3)
 Sof(S2)=FVAR(3)
 Sof(N8)=1-FVAR(4)
 Sof(S1)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C14(H14A), C9(H9), C60(H60), C65(H65)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C61(H61A,
 H61B), C64(H64A,H64B), C62(H62A,H62B), C63(H63A,H63B)
5.c Aromatic/amide H refined with riding coordinates:
 N12(H12), N11(H11), C32(H32), C30(H30), N13(H13), C29(H29), N14(H14),
 C47(H47), C54(H54), C22(H22), C38(H38), C55(H55), C71(H71), C37(H37), C34(H34),
  C69(H69), C72(H72), C20(H20), C31(H31), C46(H46), C45(H45), C44(H44),
 C19(H19), C4(H4), C57(H57), C58(H58), C68(H68), C23(H23), C35(H35), C3(H3),
 C6(H6), C7(H7), C50(H50), C51(H51), C17(H17), C18(H18)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22019
_shelx_fab_checksum              99533
_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
;