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_4337060
_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_moiety         'C28 H20 N6 Zn, 0.5(C4 H8 O2) '
_chemical_formula_sum            'C30 H24 N6 O Zn'
_chemical_formula_weight         549.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.9300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7677(4)
_cell_length_b                   8.5971(2)
_cell_length_c                   20.3458(5)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      2.41
_cell_volume                     2582.75(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80878
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.8661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       rod
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.3793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                6255
_reflns_number_total             7538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402892f_si_002_02.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4337060