From Sequential to One-Pot Synthesis of Dipyrrin Based Grid-Type Mixed Metal-Organic Frameworks
Antoine Béziau; Stéphane A. Baudron; Audrey Fluck; Mir Wais Hosseini; Inorganic Chemistry 52 (2013) 14439–14448; doi:10.1021/ic402892f

data_4337068
_publ_contact_author
; Prof Mir Wais Hosseini
  Laboratoire de Tectonique Mol\'eculaire, 
  UMR CNRS 7140, Universit\'e de Strasbourg,
  CS 90032
  F-67081 Strasbourg Cedex, France 
;
_publ_contact_author_email       hosseini@unistra.fr
_publ_contact_author_fax         '33 3 68 85 13 23'
_publ_contact_author_phone       '33 3 68 85 13 25'
_publ_section_title
;
 From Sequential to One-Pot Synthesis of Dipyrrin Based Grid-Type Mixed
 Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14439
_journal_page_last               14448
_journal_paper_doi               10.1021/ic402892f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C56 H40 Cd Cl2 Cu2 N12'
_chemical_formula_weight         1191.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           95
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw 2c'
_symmetry_space_group_name_H-M   'P 43 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0626(4)
_cell_length_b                   20.0626(4)
_cell_length_c                   19.8105(6)
_cell_measurement_reflns_used    7406
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.28
_cell_volume                     7973.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70723
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.9160
_exptl_absorpt_correction_T_min  0.8777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         9210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                6839
_reflns_number_total             9210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402892f_si_002_10.cif
_cod_data_source_block           M'MOF9
_cod_database_code               4337068