Efficient photocatalytic degradation of methyl violet using two new 3D MOFs directed by different carboxylate spacers
Wang, Jun; Rao, Congying; Lu, Lu; Zhang, Shile; Muddassir, Mohd; Liu, Jianqiang; CrystEngComm 23 (2021) 741–747; doi:10.1039/D0CE01632B

data_7241584
_publ_section_title
;
 Efficient photocatalytic degradation of methyl violet using two new 3D
 MOFs directed by different carboxylate spacers
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              741
_journal_page_last               747
_journal_paper_doi               10.1039/D0CE01632B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C75 H69 Cd3 N7 O15'
_chemical_formula_sum            'C75 H69 Cd3 N7 O15'
_chemical_formula_weight         1645.57
_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
_audit_creation_date             2019-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-05 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                97.294(3)
_cell_angle_beta                 92.079(3)
_cell_angle_gamma                109.017(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2908(5)
_cell_length_b                   15.7878(5)
_cell_length_c                   18.8266(7)
_cell_measurement_reflns_used    2585
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      41.1330
_cell_measurement_theta_min      3.8660
_cell_volume                     3969.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -114.00 -16.00   1.00    1.00    --  -40.08 -38.00 -30.00   98
  2  \w    -65.00  34.00   1.00    1.00    --  -40.08  38.00 150.00   99
  3  \w    -92.00 -42.00   1.00    1.00    --  -40.08 125.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0578110000
_diffrn_orient_matrix_UB_12      -0.1025172000
_diffrn_orient_matrix_UB_13      -0.0119931000
_diffrn_orient_matrix_UB_21      0.0644577000
_diffrn_orient_matrix_UB_22      -0.0122157000
_diffrn_orient_matrix_UB_23      0.0627328000
_diffrn_orient_matrix_UB_31      -0.0749755000
_diffrn_orient_matrix_UB_32      0.0153364000
_diffrn_orient_matrix_UB_33      0.0527450000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22447
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.537
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.668
_refine_diff_density_min         -3.075
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         13866
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1418P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9573
_reflns_number_total             13866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01632b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7241583--7241584.cif.'
_cod_original_cell_volume        3969.6(2)
_cod_database_code               7241584
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     c4a-c3-mgcl2
_shelx_estimated_absorpt_t_max   0.424
_shelx_estimated_absorpt_t_min   0.354
_reflns_odcompleteness_completeness 27.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 C(H,H,H) groups
2. Restrained distances
 O15A-C1A
 1.24 with sigma of 0.02
 C1A-N7A
 1.35 with sigma of 0.02
 N7A-C2A
 1.45 with sigma of 0.02
 C3A-N7A
 1.45 with sigma of 0.02
 O15A-N7A
 2.36 with sigma of 0.02
 C1A-C2A
 2.39 with sigma of 0.02
 C1A-C3A
 2.39 with sigma of 0.02
 C3A-C2A
 2.45 with sigma of 0.02
 O15-C73
 1.25 with sigma of 0.02
 C73-N7
 1.38 with sigma of 0.02
 N7-C74
 1.45 with sigma of 0.02
 N7-C75
 1.45 with sigma of 0.02
 N7-O15
 2.33 with sigma of 0.02
 C73-C74
 2.39 with sigma of 0.02
 C73-C75
 2.39 with sigma of 0.02
 C75-C74
 2.45 with sigma of 0.02
 C70-O14
 1.25 with sigma of 0.02
 C70-N6
 1.36 with sigma of 0.02
 C70-C72
 2.36 with sigma of 0.02
 C71-C72
 2.45 with sigma of 0.02
 C70-C71
 2.38 with sigma of 0.02
 N6-C71
 1.45 with sigma of 0.02
3. Restrained planarity
 O15A, N7A, C1A, C2A, C3A
 with sigma of 0.1
 O15, N7, C73, C74, C75
 with sigma of 0.1
 O14, N6, C70, C71, C72
 with sigma of 0.1
4. Rigid bond restraints
 O14, N6, C70, C71, C72
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O15, N7, C73, C74, O15A, N7A, C1A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O15, N7, C73, C74, C75, O15A, N7A, C1A, C2A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O14 \\sim N6 \\sim C70 \\sim C71 \\sim C72: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O15 \\sim N7 \\sim C73 \\sim C74 \\sim O15A \\sim N7A \\sim C1A \\sim C3A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O15 \\sim N7 \\sim C73 \\sim C74 \\sim C75 \\sim O15A \\sim N7A \\sim C1A \\sim
C2A \\sim C3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(O15A) \\sim Ueq, Uanis(C1A) \\sim Ueq,
Uanis(N7A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: O15(0.5) N7(0.5) C73(0.5) H73(0.5) C74(0.5) H74A(0.5) H74B(0.5)
 H74C(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) O15A(0.5) N7A(0.5) C1A(0.5)
 H1A(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5)
 H3AC(0.5)
7.a Riding coordinates:
 C55(H55A,H55B,H55C), C61(H61A,H61B,H61C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,
 H75B,H75C), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC)
7.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B), C65(H65A,H65B), C66(H66A,H66B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26), C30(H30),
  C31(H31), C33(H33), C34(H34), C36(H36), C38(H38), C40(H40), C42(H42),
 C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C52(H52), C53(H53), C57(H57),
  C58(H58), C63(H63), C64(H64), C67(H67), C70(H70), C73(H73), C1A(H1A)
;
_shelx_res_checksum              96705
_shelx_fab_checksum              90771
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.001
_oxdiff_exptl_absorpt_empirical_full_min 0.580