Construction, structures, and magnetic studies of two cobalt(ii) and nickel(ii) coordination polymers displaying bex topology
Wu, Si-Tong; Ruan, Zhijun; Tian, Zhengfang; Shi, Le; Yang, Jiong; Shao, Dong; CrystEngComm 26 (2024) 5850–5858; doi:10.1039/D4CE00935E

data_7249387
_publ_section_title
;
 Construction, structures, and magnetic studies of two cobalt(ii) and
 nickel(ii) coordination polymers displaying bex topology
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              5850
_journal_page_last               5858
_journal_paper_doi               10.1039/D4CE00935E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C11 H11 N Ni O6'
_chemical_formula_sum            'C11 H11 N Ni O6'
_chemical_formula_weight         311.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-12 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.954(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.078(2)
_cell_length_b                   9.7734(14)
_cell_length_c                   7.2286(11)
_cell_measurement_reflns_used    7165
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.42
_cell_volume                     1175.8(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9881
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.417
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1450 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.6774.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.652
_refine_diff_density_min         -2.151
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1410
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+9.1590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1363
_reflns_number_total             1410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00935e2.cif
_cod_data_source_block           Ni
_cod_depositor_comments
'Adding full bibliography for 7249387--7249388.cif.'
_cod_database_code               7249387
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.812
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C5-O2 \\sim C5-O4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq: with sigma of 0 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2)
Uanis(O2) = Uanis(O4)
4. Others
 Sof(O4)=0.5*(1-FVAR(2))
 Sof(O2)=0.5*FVAR(2)
 Fixed Sof: H4B(0.5) H4A(0.5)
5.a Rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4B,H4A)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C2(H2)
;
_shelx_res_checksum              35853
_shelx_hkl_checksum              64473
_olex2_submission_special_instructions 'No special instructions were received'