Construction of a series of pH stable Ca-based MOFs, their CO<sub>2</sub> adsorption and catalytic activity.
Bhattacharjee, Sudip; Chakraborty, Tonmoy; Banerjee, Soumadip; Das, Abhijit K.; Bhaumik, Asim; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11120–11132; doi:10.1039/d4dt01150c

data_7716271
_publ_section_title
;
 Construction of a series of pH stable Ca-based MOFs, their CO<sub>2</sub>
 adsorption and catalytic activity.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11120
_journal_page_last               11132
_journal_paper_doi               10.1039/d4dt01150c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13.05 H15.05 Ca2 N O12'
_chemical_formula_sum            'C13.05 H15.05 Ca2 N O12'
_chemical_formula_weight         458.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                96.156(8)
_cell_angle_beta                 98.994(7)
_cell_angle_gamma                113.548(7)
_cell_formula_units_Z            2
_cell_length_a                   9.2135(19)
_cell_length_b                   10.112(2)
_cell_length_c                   10.455(2)
_cell_measurement_reflns_used    5925
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      25.695
_cell_measurement_theta_min      2.236
_cell_volume                     866.3(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      166.52
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7790
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.237
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1379 before and 0.0701 after correction.
The Ratio of minimum to maximum transmission is 0.6682.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             473
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.581
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2971
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0419P)^2^+1.2637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2757
_reflns_number_total             2971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01150c2.cif
_cod_data_source_block           mo_ab170223_0m_a
_cod_depositor_comments
'Adding full bibliography for 7716268--7716271.cif.'
_cod_database_code               7716271
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.760
_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
 Ca2-H10A \\sim Ca2-H10B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11B) = Uanis(C11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C12B) = Uanis(C12A)
4. Others
 Fixed Sof: C11A(0.7) H11C(0.7) C12A(0.75) H12A(0.75) H12B(0.75) H12C(0.75)
 C13A(0.75) H13A(0.75) H13B(0.75) H13C(0.75) C11B(0.35) H11D(0.35) C12B(0.25)
 H12D(0.25) H12E(0.25) H12F(0.25) C13B(0.25) H13D(0.25) H13E(0.25) H13F(0.25)
5.a Free rotating group:
 O10(H10A,H10B)
5.b Rotating group:
 O9(H9A,H9B), O11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C11A(H11C), C11B(H11D)
5.d Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C12B(H12D,H12E,H12F), C13B(H13D,
 H13E,H13F)
;
_shelx_res_checksum              308
_olex2_submission_special_instructions 'No special instructions were received'