Crystallographic Characterization of the Metal‒Organic Framework Fe2(bdp)3 upon Reductive Cation Insertion
Biggins, Naomi; Ziebel, Michael E.; Gonzalez, Miguel; Long, Jeffrey R.; Chemical Science  (2020) –; doi:10.1039/D0SC03383A

data_1558823
_publ_section_title
;
 Crystallographic Characterization of the Metal--Organic Framework
 Fe2(bdp)3 upon Reductive Cation Insertion
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03383A
_journal_year                    2020
_chemical_formula_moiety         '0.13(C288 H192 Fe16 N96), 0.49(Na)'
_chemical_formula_sum            'C36 H24 Fe2 N12 Na0.51'
_chemical_formula_weight         748.04
_chemical_name_common            Na0.5Fe2(bdp)3
_chemical_name_systematic        Na0.5Fe2(bdp)3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-17 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.0813(16)
_cell_length_b                   26.493(7)
_cell_length_c                   45.483(12)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.41
_cell_measurement_theta_min      3.36
_cell_volume                     8533(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            42581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         31.310
_diffrn_reflns_theta_min         3.088
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1347 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.9327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3053
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3241
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+45.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2651
_reflns_number_total             3241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03383a2.cif
_cod_data_source_block           Na05Fe2(bdp)3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1558823
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C9, C10, C11, C13, C12
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 C4, C5
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9 \\sim C10 \\sim C11 \\sim C13 \\sim C12: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=1-FVAR(1)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=FVAR(1)
 Fixed Sof: C5(0.5) H5(0.5) C4(0.5) H4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C1(H1), C13(H13), C11(H11), C10(H10), C12(H12), C5(H5), C4(H4)
;
_shelx_res_checksum              6954
_olex2_submission_special_instructions 'No special instructions were received'