Iron and Porphyrin Metal‒Organic Frameworks: Insight into Structural Diversity, Stability, and Porosity
Fateeva, Alexandra; Clarisse, Jade; Pilet, Guillaume; Grenèche, Jean-Marc; Nouar, Farid; Abeykoon, Brian K.; Guegan, Frédéric; Goutaudier, Christelle; Luneau, Dominique; Warren, John E.; Rosseinsky, Matthew J.; Devic, Thomas; Crystal Growth & Design 15 (2015) 1819–; doi:10.1021/cg501855k

data_4512835
_publ_section_title
;
 Iron and Porphyrin Metal--Organic Frameworks: Insight into Structural
 Diversity, Stability, and Porosity
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1819
_journal_paper_doi               10.1021/cg501855k
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C56 H32 Fe3 N8 O8'
_chemical_formula_sum            'C56 H32 Fe3 N8 O8'
_chemical_formula_weight         1112.44
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   16.6770(7)
_cell_length_b                   16.6770(7)
_cell_length_c                   16.5322(13)
_cell_measurement_reflns_used    1903
_cell_measurement_temperature    293
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4598.0(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6805
_diffrn_reflns_theta_full        25.197
_diffrn_reflns_theta_max         29.299
_diffrn_reflns_theta_min         2.996
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.205
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9257
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         887
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.1020
_refine_ls_shift/su_max          0.0001614
_refine_ls_shift/su_mean         0.0000119
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 16.1 13.6 10.9 6.87 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1591
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.0997
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              1
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                1050
_reflns_number_total             1577
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      2.04
_oxford_refine_ls_r_factor_ref   0.0954
_oxford_refine_ls_scale          1.523(13)
_oxford_reflns_number_all        1570
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg501855k_si_004.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512834--4512837.cif.'
_cod_original_sg_symbol_H-M      'I 4/m m m '
_cod_database_code               4512835
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(15) TO N(16) 
END                                                                             
;