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_4512836
_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         'C34 H20 Fe1.5 N4 O4'
_chemical_formula_sum            'C34 H20 Fe1.5 N4 O4'
_chemical_formula_weight         632.33
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6489(9)
_cell_length_b                   16.6489(9)
_cell_length_c                   25.194(3)
_cell_measurement_reflns_used    1912
_cell_measurement_temperature    293
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     6983.4(10)
_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 0.966
_diffrn_measured_fraction_theta_max 0.889
_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  0.064
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11249
_diffrn_reflns_theta_full        25.175
_diffrn_reflns_theta_max         29.274
_diffrn_reflns_theta_min         2.853
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.715
_exptl_crystal_size_mid          0.614
_exptl_crystal_size_min          0.283
_refine_diff_density_max         1.95
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1460
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.0002124
_refine_ls_shift/su_mean         0.0000102
_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: 
 12.7 2.17 8.00 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1125
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0932
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                1623
_reflns_number_total             2413
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      1.58
_oxford_refine_ls_r_factor_ref   0.0810
_oxford_refine_ls_scale          1.550(8)
_oxford_reflns_number_all        2397
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg501855k_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512834--4512837.cif.'
_cod_original_cell_volume        6983.4(9)
_cod_original_sg_symbol_H-M      'I 4/m m m '
_cod_database_code               4512836
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (   4,X'S) H   (  41,X'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(3) TO C(4) 
U(IJ)'S  0.0, 0.010000 = C(16) TO C(2) 
U(IJ)'S  0.0, 0.010000 = C(1) TO C(2) 
U(IJ)'S  0.0, 0.010000 = C(16) TO C(3) 
END                                                                             
;