MOF transmetalation beyond cation substitution: defective distortion of IRMOF-9 in the spotlight
Canossa, Stefano; Fornasari, Luca; Demitri, Nicola; Mattarozzi, Monica; Choquesillo-Lazarte, Duane; Pelagatti, Paolo; Bacchi, Alessia; CrystEngComm 21 (2019) 827–; doi:10.1039/C8CE01808A

data_7231990
_publ_section_title
;
 MOF transmetalation beyond cation substitution: defective distortion of
 IRMOF-9 in the spotlight
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              827
_journal_paper_doi               10.1039/C8CE01808A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C54 H52 Co3 N4 O16, 3(C3 H7 N O)'
_chemical_formula_sum            'C63 H73 Co3 N7 O19'
_chemical_formula_weight         1409.07
_chemical_name_systematic
'catena-(tris(\m4-1,1'-biphenyl-4,4'-dicarboxylato)-tris-cobalt tetra(\m1-N,N-dimethylformamide)tetra(N,N-dimethylformamide) solvate'
_chemical_properties_physical    'Phase transition above 324K'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1391(7)
_cell_length_b                   13.3582(6)
_cell_length_c                   19.7524(10)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100
_cell_measurement_theta_max      33
_cell_measurement_theta_min      3
_cell_volume                     3328.0(3)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f 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  0.0585
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            135826
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.148
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1032 before and 0.0637 after correction. The Ratio of minimum to maximum transmission is 0.9152. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       plate
_exptl_crystal_F_000             1466
_exptl_crystal_preparation       'solvothermal synthesis'
_exptl_crystal_recrystallization_method 'Phase transition from another phase'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 5679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         13622
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0306P)^2^+1.1917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12322
_reflns_number_total             13622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01808a2.cif
_cod_data_source_block           CoBPDC2
_cod_depositor_comments
'Adding full bibliography for 7231989--7231991.cif.'
_cod_database_code               7231990
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.656(11)
 0.344(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C17(H17), C26(H26), C38(H38), C3(H3), C6(H6), C21(H21), C18(H18),
 C58(H58), C31(H31), C57(H57), C12(H12), C37(H37), C9(H9), C35(H35), C7(H7),
 C48(H48), C20(H20), C27(H27), C23(H23), C4(H4), C32(H32), C24(H24), C13(H13),
 C40(H40), C41(H41), C34(H34), C44(H44), C51(H51), C54(H54), C63(H63)
3.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C52(H52A,H52B,H52C), C43(H43A,H43B,H43C), C53(H53A,H53B,H53C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C45(H45A,H45B,H45C)
;
_olex2_date_sample_data_collection 2016-08-10
_olex2_exptl_crystal_mounting_method 'kapton pin'
_olex2_submission_special_instructions 'No special instructions were received'