Design and synthesis of a new family of planar and central chiral ferrocenyl phosphine ligands.
Ling, Li; Song, Zeli; Shan, He; Wang, Chao; Li, Shouting; Wang, Yanjiao; Hu, Jianfeng; Chen, Qian; Zhang, Hao; Yang, Yong; Chemical communications (Cambridge, England) 59 (2023) 2739–2742; doi:10.1039/d2cc06492h

data_7131230
_publ_section_title
;
 Design and synthesis of a new family of planar and central chiral
 ferrocenyl phosphine ligands.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2739
_journal_page_last               2742
_journal_paper_doi               10.1039/d2cc06492h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C29 H38 Fe N O2 P, C H Cl3'
_chemical_formula_sum            'C30 H39 Cl3 Fe N O2 P'
_chemical_formula_weight         638.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-01-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2416(3)
_cell_length_b                   19.7855(6)
_cell_length_c                   14.5494(4)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.53
_cell_volume                     3088.09(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62603
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.416
_diffrn_reflns_theta_min         2.528
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0576 before and 0.0508 after correction. The Ratio of minimum to maximum transmission is 0.9042. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6316
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0459P)^2^+2.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4905
_reflns_number_total             6316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06492h2.cif
_cod_data_source_block           mo_211231a_0m_a
_cod_depositor_comments
'Adding full bibliography for 7131222--7131231.cif.'
_cod_database_code               7131230
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. 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
2. Rigid bond restraints
 C6, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13, C12, C17, C16, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C10, C11, C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C11(H11), C00Y(H00Y)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C21(H21A,H21B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C5(H5), C7(H7), C4(H4), C16(H16), C15(H15), C14(H14), C9(H9),
 C2(H2), C3(H3)
3.d Fitted hexagon refined as free rotating group:
 C13(C12,C17,C16,C15,C14)
3.e Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              1433
_shelx_hkl_checksum              18741
_olex2_submission_special_instructions 'No special instructions were received'