Highly thermally stable heterogeneous catalysts: study of 0D and 3D porphyrinic MOFs
Amayuelas López, Eder; Fidalgo-Marijuan, Arkaitz; Bazán, Begoña; Urtiaga, Miren Karmele; Barandika, Gotzone; Arriortua, María Isabel; CrystEngComm  (2017) –; doi:10.1039/C7CE01702B

data_7229554
_publ_section_title
;
 Highly thermally stable heterogeneous catalysts: study of 0D and 3D
 porphyrinic MOFs
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01702B
_journal_year                    2017
_chemical_formula_moiety         'C96 H48 N8 Ni5 O20, O'
_chemical_formula_sum            'C96 H48 N8 Ni5 O21'
_chemical_formula_weight         1942.87
_chemical_name_systematic        '[Ni2.5(TCPP)(u-O)(H2O)2].nD'
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2016-05-06T13:02:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-05-09 deposited with the CCDC.
2017-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.793(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.640(4)
_cell_length_b                   33.509(2)
_cell_length_c                   16.6141(17)
_cell_measurement_reflns_used    3631
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      89.6106
_cell_measurement_theta_min      2.5775
_cell_measurement_wavelength     1.54184
_cell_volume                     9537(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2012
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0722603
_diffrn_orient_matrix_UB_12      -0.024722
_diffrn_orient_matrix_UB_13      0.0057518
_diffrn_orient_matrix_UB_21      -0.0464405
_diffrn_orient_matrix_UB_22      0.0386938
_diffrn_orient_matrix_UB_23      0.002061
_diffrn_orient_matrix_UB_31      -0.0266641
_diffrn_orient_matrix_UB_32      -0.0006444
_diffrn_orient_matrix_UB_33      -0.0953359
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1465
_diffrn_reflns_av_unetI/netI     0.101
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53209
_diffrn_reflns_theta_full        65
_diffrn_reflns_theta_max         65
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.677
_exptl_crystal_density_meas      1.546(5)
_exptl_crystal_density_method    Flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             988
_exptl_crystal_recrystallization_method Solvothermal
_exptl_crystal_size_max          0.1225
_exptl_crystal_size_mid          0.1098
_exptl_crystal_size_min          0.0229
_platon_squeeze_details
;
;
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.2919
_reflns_number_gt                3407
_reflns_number_total             7925
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7ce01702b2.cif
_cod_data_source_block           a20150133_ea630
_cod_original_cell_volume        9538(3)
_cod_database_code               7229554