Cooperative Bond Activations by a Tucked-In Iron Complex
Zurakowski, Joseph A.; Drover, Marcus W.; Chemical Communications  (2023) –; doi:10.1039/D3CC03325B

data_7132019
_publ_section_title
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 Cooperative Bond Activations by a Tucked-In Iron Complex
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03325B
_journal_year                    2023
_chemical_formula_moiety         'C24 H46 Fe P2'
_chemical_formula_sum            'C24 H46 Fe P2'
_chemical_formula_weight         452.40
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-31 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.946(9)
_cell_angle_beta                 82.104(9)
_cell_angle_gamma                77.117(8)
_cell_formula_units_Z            2
_cell_length_a                   8.3558(12)
_cell_length_b                   9.4334(16)
_cell_length_c                   16.5656(18)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.50
_cell_volume                     1255.1(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         2.225
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.9342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.6614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5346
_reflns_number_total             6237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03325b3.cif
_cod_data_source_block           2
_cod_database_code               7132019
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C14(H14A,H14B), C20(H20A,H20B), C13(H13A,H13B), C16(H16A,
 H16B), C12(H12A,H12B), C11(H11A,H11B), C17(H17A,H17B), C22(H22A,H22B),
 C23(H23A,H23B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              30768
_shelx_hkl_checksum              56709
_olex2_submission_special_instructions 'No special instructions were received'