Construction of two new Co(II)-organic frameworks based on diverse metal clusters: Highly selective C2H2 and CO2 capture and magnetic properties
Ding, Tao; Chen, Jing-Ru; Chen, Jing-Jing; Li, Zi-Yu; Gao, Dan; Zheng, Li-Na; Gao, Zi-Wei; Journal of Solid State Chemistry 305 (2022) 122629–; doi:10.1016/j.jssc.2021.122629

data_1566054
_publ_section_title
;
 Construction of two new Co(II)-organic frameworks based on diverse metal
 clusters: Highly selective C2H2 and CO2 capture and magnetic properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              122629
_journal_paper_doi               10.1016/j.jssc.2021.122629
_journal_volume                  305
_journal_year                    2022
_chemical_formula_moiety         'C45 H35 Co4 N3 O24'
_chemical_formula_sum            'C45 H35 Co4 N3 O24'
_chemical_formula_weight         1237.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 105.950(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.03(2)
_cell_length_b                   16.636(15)
_cell_length_c                   17.048(15)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.45
_cell_volume                     7644(11)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_unetI/netI     0.1384
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38863
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         0.756
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.7767.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.885
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         15448
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.1030
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2857
_refine_ls_wR_factor_ref         0.3181
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9599
_reflns_number_total             15448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2022-305-122629.cif
_cod_data_source_block           2
_cod_database_code               1566054
_exptl_absorpt_special_details   'SADABS; Bruker, 2012'
_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, All O(H,H) groups
2. Restrained distances
 O18-C41
 1.2 with sigma of 0.02
 C41-N3
 1.5 with sigma of 0.02
 N3-C42
 1.5 with sigma of 0.02
 N3-C43
 1.5 with sigma of 0.02
 C41-C42 = C42-C43 = C43-C41
 2.5 with sigma of 0.01
 O18-C41A
 1.2 with sigma of 0.02
 C41A-N3A
 1.5 with sigma of 0.02
 N3A-C43A
 1.5 with sigma of 0.02
 N3A-C42A
 1.5 with sigma of 0.02
 C42A-C43
 0.5 with sigma of 0.01
 C41A-C42A = C42A-C43A = C43A-C41A
 2.5 with sigma of 0.01
3. Restrained planarity
 C42, N3, C43, C41, O18
 with sigma of 0.1
 C41A, C42A, N3A, C43A, O18
 with sigma of 0.1
4. Rigid bond restraints
 O18, N3, C41, C42, C43, C43A, N3A, C42A, C41A
 with sigma for 1-2 distances of 0.0051 and sigma for 1-3 distances of 0.1
5. Uiso/Uaniso restraints and constraints
O18 \\sim N3 \\sim C41 \\sim C42 \\sim C43 \\sim C43A \\sim N3A \\sim C42A
\\sim C41A: within 2A with sigma of 0.0051 and sigma for terminal atoms of 0.2
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C39) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C29) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O18) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(N3A) \\sim Ueq,
Uanis(C42A) \\sim Ueq, Uanis(C41A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
6. Others
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(N3A)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=Sof(C41A)=Sof(H41A)=1-FVAR(1)
 Sof(N3)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=
 Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
7.a Riding coordinates:
 O20(H20A,H20B), C40(H40), C43A(H43D,H43E,H43F), C42A(H42D,H42E,H42F)
7.b Rotating group:
 O24(H24A,H24B), O19(H19A,H19B), O23(H23A,H23B), O21(H21A,H21B)
7.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C17(H17), C28(H28), C29(H29), C45(H45), C32(H32), C16(H16),
 C15(H15), C14(H14), C13(H13), C10(H10), C11(H11), C35(H35), C34(H34), C33(H33),
  C39(H39), C36(H36), C41(H41), C41A(H41A)
7.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;