Acid-directed synthesis of three Cd-based metal–organic frameworks with luminescence and catalytic CO2 transformation properties
Zhang, Zhen-Wei; Hu, Hui; Wang, Ming-Zhen; Zhang, Qing; Zhou, Wen-Feng; Zhang, Yan-Kai; Yang, Xin-Yi; Liu, Xue-Ying; Zhang, Yong-Zheng; Geng, Longlong; Liu, Zhong-Min; Zhang, Da-Shuai; Zhuang, Shujuan; Wei, Rong-Min; Zhang, Xiuling; CrystEngComm  (2022) –; doi:10.1039/D2CE01327D

data_7245926
_publ_section_title
;
 Acid-directed synthesis of three Cd-based metal--organic frameworks with
 luminescence and catalytic CO2 transformation properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01327D
_journal_year                    2022
_chemical_formula_moiety
'0.25(C316 H220 Cd16 N24 O84), 2(C2 H5 O), 2(H2 O)'
_chemical_formula_sum            'C83 H69 Cd4 N6 O25'
_chemical_formula_weight         2000.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-19 deposited with the CCDC.	2022-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.729(2)
_cell_length_b                   21.126(3)
_cell_length_c                   21.855(3)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.782
_cell_measurement_theta_min      2.189
_cell_volume                     8185.6(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.162
_diffrn_reflns_theta_min         1.765
_exptl_absorpt_coefficient_mu    1.107
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             4004
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10026
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0645P)^2^+31.0128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6886
_reflns_number_total             10026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01327d2.cif
_cod_data_source_block           3
_cod_database_code               7245926
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C35-C36 = N2-C37
 2.3 with sigma of 0.02
3. Rigid bond restraints
 C33, C34, C35, N1, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, C43, C44, N3, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.2
Uanis(N3) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.2
5. Others
 Fixed Sof: C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5) C40(0.5)
 C41(0.5) H41(0.5) C36(0.5) C37(0.5) H37(0.5) C38(0.5) C39(0.5) H39(0.5)
 C45(0.5) H45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5) N1(0.5) N2(0.5) N3(0.5)
 C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) N4(0.5) N5(0.5) N6(0.5)
 H6a(0.5) O11(0.5) H11a(0.5) H11b(0.5)
6.a Riding coordinates:
 O12(H12a,H12b)
6.b Rotating group:
 O9(H9a,H9b), O10(H10a,H10b), O11(H11a,H11b)
6.c :
 C40(C41,C36,C37,C38,C39), N3(C42,C43,C44,N4)
6.d Ternary CH refined with riding coordinates:
 C41(H41)
6.e Me refined with riding coordinates:
 C49(H49a,H49b,H49c)
6.f Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C20(H20), C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30),
  C33(H33), C34(H34), C35(H35), C37(H37), C39(H39), C45(H45), C46(H46),
 C47(H47), C42(H42), C43(H43), C44(H44), N6(H6a), C48(H48)
6.g Idealised tetrahedral OH refined as rotating group:
 O13(H13a)
;
_shelx_res_checksum              85357
_shelx_hkl_checksum              84455
_shelx_fab_checksum              17039
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'