Synthesis and characterization of enantiopure planar‒chiral phosphorus-linked diferrocenes
Honegger, Philipp; Roller, Alexander; Widhalm, Michael; Acta Crystallographica Section C 77 (2021) 152–160; doi:10.1107/S2053229621001996

data_2022332
_publ_section_title
;
 Synthesis and characterization of enantiopure planar--chiral
 phosphorus-linked diferrocenes
;
_journal_coeditor_code           ZO3008
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              152
_journal_page_last               160
_journal_paper_doi               10.1107/S2053229621001996
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Fe2 (C5 H5)2 (C22 H21 O2 P S)]'
_chemical_formula_moiety         'C32 H31 Fe2 O2 P S'
_chemical_formula_sum            'C32 H31 Fe2 O2 P S'
_chemical_formula_weight         622.30
_chemical_name_common            monohydroxymonoacetatephosphinesulfide
_chemical_name_systematic
'{(2<i>S</i>~p~)-2-[(1<i>R</i>)-1-(Acetyloxy)ethyl]ferrocen-1-yl}[(2<i>S</i>~p~)-2-ethenylferrocen-1-yl]phenyl-(<i>S</i>)-phosphane sulfide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4923(3)
_cell_length_b                   12.0133(4)
_cell_length_c                   31.7580(10)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.593
_cell_measurement_theta_min      2.563
_cell_volume                     2858.45(17)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            52739
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.024
_diffrn_reflns_theta_min         2.564
_diffrn_source                   'sealed xray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.342
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2809 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         8330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0231P)^2^+0.8513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                7214
_reflns_number_total             8330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3008sup1.cif
_cod_data_source_block           8a
_cod_depositor_comments
'Adding full bibliography for 2022331--2022336.cif.'
_cod_database_code               2022332
_cod_database_fobs_code          2022332
_shelx_estimated_absorpt_t_min   0.793
_shelx_estimated_absorpt_t_max   0.944
_shelx_hkl_checksum              2335
_shelx_res_checksum              45110