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_7241253
_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         '2(C9.5 H8 Co0.25 N O1.5)'
_chemical_formula_sum            'C19 H16 Co0.5 N2 O3'
_chemical_formula_weight         349.80
_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                88.1580(10)
_cell_angle_beta                 75.0940(10)
_cell_angle_gamma                86.4140(10)
_cell_formula_units_Z            8
_cell_length_a                   15.2700(2)
_cell_length_b                   15.73680(10)
_cell_length_c                   17.1187(2)
_cell_measurement_reflns_used    36485
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.7630
_cell_measurement_theta_min      2.6600
_cell_volume                     3966.88(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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     41.00 104.00   0.50    0.79    --   48.05  73.00-110.00  126
  2  \w    145.00 170.00   0.50    3.16    --  107.75  73.00-110.00   50
  3  \w    128.00 176.00   0.50    3.16    --  107.75  61.00 -30.00   96
  4  \w    153.00 178.00   0.50    3.16    --  107.75  45.00   0.00   50
  5  \w    141.00 166.00   0.50    3.16    --  107.75  15.00  60.00   50
  6  \w    114.00 157.00   0.50    3.16    --  107.75  45.00 150.00   86
  7  \w     98.00 132.00   0.50    3.16    --  107.75  15.00  60.00   68
  8  \w     99.00 149.00   0.50    3.16    --  107.75  45.00   0.00  100
  9  \w     98.00 178.00   0.50    3.16    --  107.75  15.00 -90.00  160
 10  \w    127.00 159.00   0.50    3.16    --  107.75   0.00-120.00   64
 11  \w     98.00 177.00   0.50    3.16    --  107.75  15.00 -60.00  158
 12  \w    109.00 162.00   0.50    3.16    --  107.75 125.00-180.00  106
 13  \w     36.00 110.00   0.50    3.16    --  107.75   0.00-120.00  148
 14  \w     77.00 106.00   0.50    3.16    --  107.75 -94.00   0.00   58
 15  \w     79.00 106.00   0.50    3.16    --  107.75 -94.00 -30.00   54
 16  \w     79.00 106.00   0.50    3.16    --  107.75 -94.00 -90.00   54
 17  \w     73.00 108.00   0.50    3.16    --  107.75-125.00 -90.00   70
 18  \w     44.00  98.00   0.50    3.16    --  107.75-125.00   0.00  108
 19  \w     48.00  74.00   0.50    3.16    --  107.75 -94.00 -90.00   52
 20  \w     48.00 106.00   0.50    3.16    --  107.75 -94.00-150.00  116
 21  \w     36.00  66.00   0.50    3.16    --  107.75 -61.00 -30.00   60
 22  \w     47.00  74.00   0.50    3.16    --  107.75 -77.00   0.00   54
 23  \w     51.00 105.00   0.50    3.16    --  107.75 -94.00  30.00  108
 24  \w     78.00 108.00   0.50    3.16    --  107.75-107.00 115.96   60
 25  \w     70.00 105.00   0.50    3.16    --  107.75 -94.00  90.00   70
 26  \w     53.00 102.00   0.50    3.16    --  107.75 -94.00 150.00   98
 27  \w     39.00  65.00   0.50    3.16    --  107.75 -73.00 120.00   52
 28  \w     38.00  77.00   0.50    3.16    --  107.75 -94.00 120.00   78
 29  \w     41.00 107.00   0.50    3.16    --  107.75-125.00 120.00  132
 30  \w     38.00  64.00   0.50    3.16    --  107.75 -94.00  90.00   52
 31  \w     36.00  90.00   0.50    3.16    --  107.75-125.00  90.00  108
 32  \w     36.00 109.00   0.50    3.16    --  107.75-115.00   2.00  146
 33  \w     45.00 105.00   0.50    3.16    --  107.75 -97.00-104.24  120
 34  \w     36.00  69.00   0.50    3.16    --  107.75 -61.00-180.00   66
 35  \w     38.00 106.00   0.50    3.16    --  107.75 -94.00-180.00  136
 36  \w     37.00  63.00   0.50    3.16    --  107.75 -61.00-150.00   52
 37  \w     36.00  75.00   0.50    3.16    --  107.75 -77.00 -90.00   78
 38  \w     38.00  69.00   0.50    3.16    --  107.75 -61.00 -90.00   62
 39  \w     34.00  94.00   0.50    0.79    --   48.05-125.00   0.00  120
 40  \w     38.00  64.00   0.50    3.16    --  107.75 -77.00  90.00   52
 41  \w     38.00  69.00   0.50    3.16    --  107.75 -61.00 150.00   62
 42  \w     36.00 106.00   0.50    3.16    --  107.75 -99.00 151.61  140
 43  \w    -20.00  67.00   0.50    0.79    --   48.05 -73.00 120.00  174
 44  \w    -17.00  22.00   0.50    0.79    --  -48.05  19.00 -60.00   78
 45  \w    -29.00  -3.00   0.50    0.79    --  -48.05  19.00-150.00   52
 46  \w    -28.00  16.00   0.50    0.79    --  -48.05  19.00-180.00   88
 47  \w    -68.00  23.00   0.50    0.79    --  -48.05  73.00-110.00  182
 48  \w    -46.00 -14.00   0.50    3.16    --  -86.25  45.00  60.00   64
 49  \w    -50.00 -16.00   0.50    3.16    --  -86.25  45.00  90.00   68
 50  \w    -68.00 -14.00   0.50    0.79    --  -48.05 125.00 150.00  108
 51  \w    -77.00 -52.00   0.50    3.16    --  -86.25  73.00-110.00   50
 52  \w    -97.00 -38.00   0.50    0.79    --  -48.05 -73.00 120.00  118
 53  \w     95.00 148.00   0.50    3.16    --  107.75 125.00 150.00  106
 54  \w   -119.00 -74.00   0.50    0.79    --  -48.05-125.00-120.00   90
 55  \w   -136.00-111.00   0.50    3.16    --  -86.25 -73.00 120.00   50
;
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67368
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.096
_diffrn_reflns_theta_min         2.671
_exptl_absorpt_coefficient_mu    3.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       plate
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.091(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1766
_refine_ls_number_reflns         21540
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+4.9869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                19607
_reflns_number_total             21540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01172j2.cif
_cod_data_source_block           compound_3
_cod_original_formula_sum        'C19 H16 Co0.50 N2 O3'
_cod_database_code               7241253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.285
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.909(4)
 0.091(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3.a Ternary CH refined with riding coordinates:
 C117(H117), C122(H122), C139(H139), C46(H46), C64(H64), C63(H63), C41(H41),
 C144(H144)
3.b Secondary CH2 refined with riding coordinates:
 C140(H14B,H14C), C67(H67A,H67B), C43(H43A,H43B), C141(H14D,H14E), C119(H11B,
 H11C), C121(H12A,H12B), C42(H42A,H42B), C120(H12C,H12D), C44(H44A,H44B),
 C68(H68A,H68B), C65(H65A,H65B), C118(H11D,H11E), C45(H45A,H45B), C142(H14F,
 H14G), C66(H66A,H66B), C143(H14H,H14I)
3.c Aromatic/amide H refined with riding coordinates:
 N15(H15A), C16(H16), N11(H11), N13(H13), N10(H10A), N12(H12), N14(H14),
 C60(H60), N16(H16A), C93(H93), C32(H32), C14(H14A), C94(H94), N9(H9),
 C100(H100), C78(H78), C13(H13A), C89(H89), C102(H102), C129(H129), C86(H86),
 C74(H74), C1(H1), C29(H29), C58(H58), C31(H31), C103(H103), C61(H61), C4(H4),
 C96(H96), C128(H128), C150(H150), C80(H80), C11(H11A), C111(H111), C15(H15),
 C18(H18), C97(H97), C27(H27), C23(H23), C26(H26), C50(H50), C137(H137),
 C53(H53), C10(H10), C57(H57), C83(H83), C77(H77), C133(H133), C75(H75),
 C24(H24), C30(H30), C115(H115), C136(H136), C99(H99), C125(H125), C148(H148),
 C107(H107), C108(H108), C17(H17), C2(H2), C84(H84), C147(H147), C91(H91),
 C7(H7), C87(H87), C8(H8), C52(H52), C126(H126), C90(H90), C49(H49), C134(H134),
  C72(H72), C20(H20), C21(H21), C81(H81), C114(H114), C5(H5), C71(H71),
 C106(H106), C92(H92), C112(H112), C151(H151), C35(H35), C105(H105), C36(H36),
 C39(H39), C38(H38)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26926
_shelx_fab_checksum              83517
_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
;