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_1558822
_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), 4(C0.86 H2 N0.29 O0.29)'
_chemical_formula_sum            'C39.44 H32.02 Fe2 N13.14 O1.15'
_chemical_formula_weight         820.08
_chemical_name_common            Fe2(bdp)3(DMF)0.58
_chemical_name_systematic        Fe2(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
_audit_creation_date             2019-09-18
_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                   7.0648(4)
_cell_length_b                   26.4382(14)
_cell_length_c                   45.215(3)
_cell_measurement_reflns_used    5036
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.74
_cell_measurement_theta_min      3.76
_cell_volume                     8445.3(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            22769
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.981
_diffrn_reflns_theta_max         30.981
_diffrn_reflns_theta_min         2.224
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1389 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.8053.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3374
_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_refine_diff_density_max         2.622
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1749
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0718
_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^)+(0.1139P)^2^+128.2064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1428
_reflns_number_total             1749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03383a2.cif
_cod_data_source_block           Fe2(bdp)3
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1558822
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N4-C14
 1.327 with sigma of 0.06
 C14-O1
 1.231 with sigma of 0.06
 N4-C15
 1.44 with sigma of 0.05
 C16-N4
 1.441 with sigma of 0.05
 C15-C14
 2.41 with sigma of 0.08
 C16-C14
 2.41 with sigma of 0.08
3. Restrained planarity
 C15, N4, C16, C14
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C5 \\sim C4 \\sim C13 \\sim C11 \\sim C10 \\sim C12: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
O1 \\sim C14 \\sim N4 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C5, C4, C11, C10, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, N4, C16, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H16C)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(H16B)=Sof(H16A)=Sof(H15F)=
 Sof(H15A)=Sof(H15C)=Sof(H15B)=Sof(H15E)=Sof(H15D)=0.5*FVAR(2)
 Sof(C16)=Sof(N4)=Sof(C14)=Sof(H14)=Sof(O1)=Sof(C15)=FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=1-FVAR(2)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=FVAR(2)
 Fixed Sof: C5(0.5) H5(0.5) C4(0.5) H4(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C1(H1), C12(H12), C5(H5), C11(H11), C13(H13), C10(H10),
 C4(H4), C14(H14)
7.b Disordered Me refined with riding coordinates:
 C16(H16C,H16D,H16E,H16F,H16B,H16A), C15(H15F,H15A,H15C,H15B,H15E,H15D)
;
_shelx_res_checksum              49392
_olex2_submission_special_instructions 'No special instructions were received'