Tuning the iron redox state inside a microporous porphyrinic metal organic framework.
Abeykoon, Brian; Grenèche, Jean-Marc; Jeanneau, Erwann; Chernyshov, Dmitry; Goutaudier, Christelle; Demessence, Aude; Devic, Thomas; Fateeva, Alexandra; Dalton transactions (Cambridge, England : 2003) 46 (2017) 517–523; doi:10.1039/c6dt04208b

data_7041360
_publ_section_title
;
 Tuning the iron redox state inside a microporous porphyrinic metal
 organic framework.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              517
_journal_page_last               523
_journal_paper_doi               10.1039/c6dt04208b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C14 H12 Fe0.75 N5.50 O0.50'
_chemical_formula_sum            'C14 H12 Fe0.75 N5.5 O0.5'
_chemical_formula_weight         307.17
_space_group_IT_number           65
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-11-03 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.160(2)
_cell_length_b                   34.398(11)
_cell_length_c                   19.626(4)
_cell_measurement_reflns_used    1960
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.6310
_cell_measurement_theta_min      3.3760
_cell_volume                     4834(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12454
_diffrn_reflns_theta_full        26.371
_diffrn_reflns_theta_max         29.396
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    0.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
;
_refine_diff_density_max         2.14
_refine_diff_density_min         -2.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3326
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.0058851
_refine_ls_shift/su_mean         0.0000611
_refine_ls_structure_factor_coef Fsqd
_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: 
 245. 375. 186. 46.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2757
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2757
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              45
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2074
_reflns_number_total             3339
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.49
_oxford_diffrn_Wilson_scale      7.25
_oxford_refine_ls_r_factor_ref   0.1240
_oxford_refine_ls_scale          0.567(3)
_oxford_reflns_number_all        3326
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c6dt04208b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7041360--7041361.cif.'
_cod_original_sg_symbol_H-M      'C m m m '
_cod_original_formula_sum        'C14 H12 Fe0.75 N5.50 O0.50'
_cod_database_code               7041360
_oxdiff_exptl_absorpt_empirical_full_min 0.841
_oxdiff_exptl_absorpt_empirical_full_max 1.185
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;