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_7231989
_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         'C24 H19 Co1.5 N O7'
_chemical_formula_sum            'C24 H19 Co1.5 N O7'
_chemical_formula_weight         521.80
_chemical_name_systematic
'catena-(tris(\m4-1,1'-biphenyl-4,4'-dicarboxylato)-tris-cobalt bis(N,N-dimethylformamide)'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.256(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0222(14)
_cell_length_b                   15.1754(19)
_cell_length_c                   19.331(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    353
_cell_measurement_theta_max      33
_cell_measurement_theta_min      3
_cell_volume                     3181.8(8)
_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      353.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0834 before and 0.0542 after correction. The Ratio of minimum to maximum transmission is 0.7741. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       prism
_exptl_crystal_F_000             1066
_exptl_crystal_preparation       'Solvothermal synthesis'
_exptl_crystal_recrystallization_method 'Solvothermal reaction'
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0378P)^2^+2.5023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4354
_reflns_number_total             5397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01808a2.cif
_cod_data_source_block           CoBPDC1
_cod_depositor_comments
'Adding full bibliography for 7231989--7231991.cif.'
_cod_original_cell_volume        3181.7(7)
_cod_original_formula_sum        'C24 H19 Co1.50 N O7'
_cod_database_code               7231989
_shelx_shelxl_version_number     2014/7
_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
2. Others
 Fixed Sof: C6(0.5) H6(0.5) C1(0.5) H1(0.5) C4(0.5) H4(0.5) C3(0.5) H3(0.5)
 C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C1A(0.5) H1A(0.5) C6A(0.5) H6A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C20(H20), C19(H19), C10(H10), C11(H11), C13(H13),
 C14(H14), C22(H22), C6(H6), C1(H1), C4(H4), C3(H3), C3A(H3A), C4A(H4A),
 C1A(H1A), C6A(H6A)
3.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C)
;
_olex2_date_sample_data_collection 2016-08-04
_olex2_exptl_crystal_mounting_method 'kapton pin'
_olex2_submission_special_instructions 'No special instructions were received'