Rational synthesis, crystal structure, and sensing and adsorption properties of luminescent metal‒organic frameworks
Fan, Chuanbin; Zong, Ziao; Meng, Xiangmin; Zhang, Xia; Zhang, Xiaoyin; Zhang, Dongmei; Xu, Cungang; Wang, Hu; Fan, Yuhua; CrystEngComm 21 (2019) 4880–; doi:10.1039/C9CE00545E

data_7234929
_publ_section_title
;
 Rational synthesis, crystal structure, and sensing and adsorption
 properties of luminescent metal--organic frameworks
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4880
_journal_paper_doi               10.1039/C9CE00545E
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C33 H22 Cd N4 O8'
_chemical_formula_sum            'C33 H22 Cd N4 O8'
_chemical_formula_weight         714.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-10-19 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6398(8)
_cell_length_b                   12.1917(11)
_cell_length_c                   25.562(2)
_cell_measurement_reflns_used    3412
_cell_measurement_temperature    173
_cell_measurement_theta_max      21.371
_cell_measurement_theta_min      2.647
_cell_volume                     3004.2(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16611
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.116
_diffrn_reflns_theta_min         1.593
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0730 before and 0.0561 after correction. The Ratio of minimum to maximum transmission is 0.8868. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1917 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     431
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0180P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                5150
_reflns_number_total             5868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00545e2.cif
_cod_data_source_block           zz
_cod_original_cell_volume        3004.2(5)
_cod_database_code               7234929
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O3-C1 \\sim O2-C1
 with sigma of 0.02
 O2-C1 \\sim O3-C1
 with sigma of 0.02
 C4-C2AA \\sim C4-C0AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.005 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(O8) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O10(0.5) H10(0.5) O9(0.5) O2(0.4) O3(0.6) O8(0.5) H8(0.5) O11(0.5)
 C0AA(0.5) C2AA(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
6.b Idealised tetrahedral OH refined as rotating group:
 O10(H10), O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'