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_4512837
_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         'C51 H34 Cs1 Fe2 N5 O11'
_chemical_formula_sum            'C51 H34 Cs Fe2 N5 O11'
_chemical_formula_weight         1137.46
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 91.637(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   7.4416(5)
_cell_length_b                   24.8056(16)
_cell_length_c                   30.314(2)
_cell_measurement_reflns_used    6765
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     5593.5(6)
_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 0.976
_diffrn_measured_fraction_theta_max 0.928
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            18836
_diffrn_reflns_theta_full        25.221
_diffrn_reflns_theta_max         29.327
_diffrn_reflns_theta_min         2.859
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.39
_refine_diff_density_min         -4.125
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0806
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4408
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.1010
_refine_ls_shift/su_max          0.0001356
_refine_ls_shift/su_mean         0.0000106
_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: 
 3.31 0.859 1.98 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1218
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1000
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                4970
_reflns_number_total             6671
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.22
_oxford_diffrn_Wilson_scale      19.24
_oxford_refine_ls_r_factor_ref   0.0929
_oxford_refine_ls_scale          0.3546(12)
_oxford_reflns_number_all        6622
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg501855k_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512834--4512837.cif.'
_cod_original_cell_volume        5593.4(6)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C51 H34 Cs1 Fe2 N5 O11'
_cod_database_code               4512837
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONTINUE CS(1,U'S) UNTIL O(39) 
CONTINUE N(1,U[ISO]) UNTIL C(1) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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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(36) TO O(38) 
DISTANCE 1.500000 , 0.001000 = N(1) TO C(1) 
DISTANCE 1.500000 , 0.010000 = N(1) TO C(2) 
DISTANCE 1.500000 , 0.010000 = N(1) TO C(3) 
DISTANCE 1.200000 , 0.001000 = O(14) TO C(1) 
U(IJ)'S  0.0, 0.001000 = O(14) TO C(1) 
U(IJ)'S  0.0, 0.001000 = FE(18) TO O(39) 
ANGLE 120.000000 , 1.000000 = C(3) TO N(1) TO C(2) 
ANGLE 120.000000 , 1.000000 = C(3) TO N(1) TO C(1) 
ANGLE 120.000000 , 1.000000 = C(1) TO N(1) TO C(2) 
ANGLE 120.000000 , 1.000000 = N(1) TO C(1) TO O(14) 
END                                                                             
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