Synthesis and coordination of hybrid phosphinoferrocenes with extended donor pendants
Navratil, Michal; Cisarova, Ivana; Štěpnička, Petr; Dalton Transactions  (2022) –; doi:10.1039/D2DT02514K

data_7711189
_publ_section_title
;
 Synthesis and coordination of hybrid phosphinoferrocenes with extended
 donor pendants
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02514K
_journal_year                    2022
_chemical_formula_moiety         'C36 H33 Cl Fe N P2 Pd, F6 Sb, C3 H6 O'
_chemical_formula_sum            'C39 H39 Cl F6 Fe N O P2 Pd Sb'
_chemical_formula_weight         1033.10
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-07-23 deposited with the CCDC.	2022-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6187(6)
_cell_length_b                   15.7642(10)
_cell_length_c                   23.9021(16)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.35
_cell_volume                     3914.5(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'PLATON (Spek, 2017)'
_computing_publication_material  'PLATON (Spek, 2017)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            223757
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         1.973
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.067
_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     532
_refine_ls_number_reflns         9004
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0048P)^2^+6.9766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8406
_reflns_number_total             9004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02514k3.cif
_cod_data_source_block           mn451
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711189
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.379
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              20645
_shelx_hkl_checksum              67002