Contorting the hetero phosphaquinoid: synthesis and electronic insights into a non-planar, ferrocenyl phosphaquinoid.
Deka, Rajesh; Chattopadhyay, Samir; Orthaber, Andreas; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3113–3117; doi:10.1039/d4dt03542a

data_7717856
_publ_section_title
;
 Contorting the hetero phosphaquinoid: synthesis and electronic insights
 into a non-planar, ferrocenyl phosphaquinoid.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3113
_journal_page_last               3117
_journal_paper_doi               10.1039/d4dt03542a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C49 H51 Fe P'
_chemical_formula_sum            'C49 H51 Fe P'
_chemical_formula_weight         726.71
_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             2024-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-23 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                104.924(7)
_cell_angle_beta                 100.810(6)
_cell_angle_gamma                97.855(7)
_cell_formula_units_Z            2
_cell_length_a                   10.741(4)
_cell_length_b                   11.706(4)
_cell_length_c                   17.303(6)
_cell_measurement_reflns_used    1333
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      17.21
_cell_measurement_theta_min      2.42
_cell_volume                     2025.3(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.1965
_diffrn_reflns_av_unetI/netI     0.3073
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19945
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.836
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1635 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.5889.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       plate
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.3005
_refine_ls_R_factor_gt           0.1588
_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^)+(0.0746P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2832
_reflns_number_total             6590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03542a2.cif
_cod_data_source_block           ao_rd_fcph_pc_brown_1_0m
_cod_depositor_comments
'Adding full bibliography for 7717855--7717856.cif.'
_cod_database_code               7717856
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.936
_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. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C8(H8), C30(H30), C6(H6), C5(H5), C22(H22), C4(H4), C17(H17),
 C7(H7), C19(H19), C3(H3), C27(H27), C13(H13), C21(H21), C20(H20), C1(H1),
 C23(H23), C2(H2), C26(H26), C16(H16), C15(H15), C14(H14), C24(H24), C25(H25)
3.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C41(H41A,H41B,H41C), C40(H40A,
 H40B,H40C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              66620
_olex2_submission_special_instructions 'No special instructions were received'