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_7129600
_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 H31 Cl Fe P2'
_chemical_formula_sum            'C20 H31 Cl Fe P2'
_chemical_formula_weight         424.68
_chemical_name_systematic        FeCp*(dvpe)Cl
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-02-23
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2021-10-22 deposited with the CCDC.	2022-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.0479(7)
_cell_length_b                   28.4512(13)
_cell_length_c                   18.5315(9)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      42.132
_cell_measurement_theta_min      4.772
_cell_volume                     8461.1(7)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex Duo II'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            54259
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        42.195
_diffrn_reflns_theta_max         42.195
_diffrn_reflns_theta_min         2.384
_exptl_absorpt_coefficient_mu    8.286
_exptl_absorpt_correction_T_max  0.7483
_exptl_absorpt_correction_T_min  0.4783
_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 0.1351 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.6392.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(5)
_refine_ls_extinction_coef       0.000025(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         5827
_refine_ls_number_restraints     1023
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+36.1041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4725
_reflns_number_total             5827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07060f3.cif
_cod_data_source_block           nix2
_cod_depositor_comments
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2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C80 H124 Cl4 Fe4 P8'
_cod_original_formula_weight         1698.74
_cod_original_formula_moiety         '4(C20 H31 Cl Fe P2)'
_cod_original_formula_units_Z            4
_cod_database_code               7129600
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.473(17)
 0.527(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C13-C14
 1.28 with sigma of 0.02
 C15-C16
 1.28 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C31(H31A,H31B), C32(H32A,H32B), C51(H51A,
 H51B), C52(H52A,H52B), C71(H71A,H71B), C72(H72A,H72B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C13(H13), C15(H15), C33(H33), C35(H35), C37(H37),
 C39(H39), C53(H53), C55(H55), C57(H57), C59(H59), C73(H73), C75(H75), C77(H77),
  C79(H79)
5.c X=CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C14(H14A,H14B), C16(H16A,H16B), C34(H34A,
 H34B), C36(H36A,H36B), C38(H38A,H38B), C40(H40A,H40B), C54(H54A,H54B),
 C56(H56A,H56B), C58(H58A,H58B), C60(H60A,H60B), C74(H74A,H74B), C76(H76A,H76B),
  C78(H78A,H78B), C80(H80A,H80B)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C)
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_shelx_res_checksum              40661
_olex2_submission_special_instructions 'No special instructions were received'