Controllable assembly over two CoII-based coordination polymers: structures and catalytic properties towards the alkene oxyalkylation reaction
Xu, Li-Mei; Wang, Qian; Zhang, Lin; Shen, Jin-Qiu; Chen, Xiao-Lu; Zhang, Jian-Yong; Liu, Zhen-Jiang; CrystEngComm 26 (2024) 6134–6142; doi:10.1039/D4CE00857J

data_7249366
_publ_section_title
;
 Controllable assembly over two CoII-based coordination polymers:
 structures and catalytic properties towards the alkene oxyalkylation
 reaction
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6134
_journal_page_last               6142
_journal_paper_doi               10.1039/D4CE00857J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C32 H24 Br Co N3 O4, 20[H2O]'
_chemical_formula_sum            'C32 H64 Br Co N3 O24'
_chemical_formula_weight         1013.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-26 deposited with the CCDC.	2024-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1870(6)
_cell_length_b                   14.6764(6)
_cell_length_c                   23.0468(9)
_cell_measurement_reflns_used    6576
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      75.1780
_cell_measurement_theta_min      3.4590
_cell_volume                     5136.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.944
_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    -22.00   3.00   0.50    0.10    --   47.70  -6.00 114.00   50
  2  \w     37.00  68.00   0.50    0.40    --  106.49 -61.00 120.00   62
  3  \w    116.00 169.00   0.50    0.40    --  106.49  30.00   0.00  106
  4  \w    111.00 155.00   0.50    0.40    --  106.49 124.00  65.00   88
  5  \w    -17.00  10.00   0.50    0.10    --   47.70 -19.00-120.00   54
  6  \w    -27.00  18.00   0.50    0.10    --  -47.70  19.00 -90.00   90
  7  \w    -75.00 -49.00   0.50    0.10    --  -47.70 125.00  30.00   52
  8  \w    -91.00 -44.00   0.50    0.40    --  -86.25 134.00 -29.00   94
  9  \w    -42.00  26.00   0.50    0.10    --  -47.70  37.00  30.00  136
 10  \w   -150.00 -63.00   0.50    0.40    --  -86.25  -6.00 114.00  174
 11  \w   -119.00 -94.00   0.50    0.10    --  -47.70-125.00-150.00   50
 12  \w     36.00 110.00   0.50    0.40    --  106.49-125.00  90.00  148
 13  \w     72.00 109.00   0.50    0.40    --  106.49-125.00 120.00   74
 14  \w     35.00  68.00   0.50    0.40    --  106.49-125.00 120.00   66
 15  \w     76.00 101.00   0.50    0.40    --  106.49-125.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0374374000
_diffrn_orient_matrix_UB_12      -0.0078471000
_diffrn_orient_matrix_UB_13      0.0619039000
_diffrn_orient_matrix_UB_21      -0.0943761000
_diffrn_orient_matrix_UB_22      -0.0020286000
_diffrn_orient_matrix_UB_23      0.0245224000
_diffrn_orient_matrix_UB_31      -0.0007168000
_diffrn_orient_matrix_UB_32      -0.1046392000
_diffrn_orient_matrix_UB_33      -0.0051831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21937
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.881
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
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    1.311
_exptl_crystal_description       rod
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00050(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0610
_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/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3844
_reflns_number_total             5331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00857j2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7249365--7249366.cif.'
_cod_database_code               7249366
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C9(0.5) H9(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C10(H10)
3.b Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18)
;
_shelx_res_checksum              43367
_shelx_hkl_checksum              43522
_shelx_fab_checksum              92613
_platon_squeeze_void_probe_radius 1.20
_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 2.406
_oxdiff_exptl_absorpt_empirical_full_min 0.651