Zero valent iron complexes as base partners in frustrated Lewis pair chemistry.
Tinnermann, Hendrik; Fraser, Craig; Young, Rowan D.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15184–15189; doi:10.1039/d0dt03551c

data_7706285
_publ_section_title
;
 Zero valent iron complexes as base partners in frustrated Lewis pair
 chemistry.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15184
_journal_page_last               15189
_journal_paper_doi               10.1039/d0dt03551c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C9 H19 Fe O3 P2, C36 H B2 F30 O, C6 H5.5 F0.5'
_chemical_formula_sum            'C51 H25.5 B2 F30.5 Fe O4 P2'
_chemical_formula_weight         1421.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                84.826(2)
_cell_angle_beta                 83.992(3)
_cell_angle_gamma                80.351(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4374(9)
_cell_length_b                   14.0427(9)
_cell_length_c                   15.3107(10)
_cell_measurement_reflns_used    9388
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.42
_cell_measurement_theta_min      2.77
_cell_volume                     2614.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.92
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59794
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.663
_diffrn_reflns_theta_min         2.726
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1033 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.8482. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.379
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         22246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+1.8115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15738
_reflns_number_total             22246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03551c2.cif
_cod_data_source_block           mo_ry_ht_1_380_0m
_cod_original_formula_sum        'C51 H25.50 B2 F30.50 Fe O4 P2'
_cod_database_code               7706285
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H46(0.5) F31(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C48(H48), C49(H49), C47(H47), C51(H51), C46(H46), C50(H50)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              9739
_olex2_submission_special_instructions 'No special instructions were received'