Bis(1-Bora-4-phosphorinane) Ring Closure at Cp*M (M = Fe, Co) Complexes
Zurakowski, Joseph A.; Austen, Brady; Brown, Kasey C.; Drover, Marcus W.; Chemical Communications  (2022) –; doi:10.1039/D1CC07060F

data_7129598
_publ_section_title
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 Bis(1-Bora-4-phosphorinane) Ring Closure at Cp*M (M = Fe, Co) Complexes
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07060F
_journal_year                    2022
_chemical_formula_moiety         'C20 H32 Cl2 Fe P4'
_chemical_formula_sum            'C20 H32 Cl2 Fe P4'
_chemical_formula_weight         523.08
_chemical_name_systematic        'Compound 5'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-20
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497)
;
_audit_update_record
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2021-10-22 deposited with the CCDC.	2022-01-20 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 110.928(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9554(5)
_cell_length_b                   11.4309(6)
_cell_length_c                   12.4135(9)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      39.047
_cell_measurement_theta_min      3.018
_cell_volume                     1186.92(13)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         39.891
_diffrn_reflns_theta_min         2.502
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0713 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.9196.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         7170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0265P)^2^+0.5424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5534
_reflns_number_total             7170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07060f3.cif
_cod_data_source_block           p17382
_cod_database_code               7129598
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9)
2.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C8(H8A,H8B), C10(H10A,H10B)
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_olex2_submission_special_instructions 'No special instructions were received'