Synthesis of Pt(ii) phosphinocarboxylate complexes with auxiliary arylcarbene ligands and factors that control their stereochemistry
Horký, Filip; Soellner, Johannes; Schulz, Jiří; Císařová, Ivana; Strassner, Thomas; Štěpnička, Petr; New Journal of Chemistry 47 (2023) 18442–18449; doi:10.1039/D3NJ03729K

data_7062734
_publ_section_title
;
 Synthesis of Pt(ii) phosphinocarboxylate complexes with auxiliary
 arylcarbene ligands and factors that control their stereochemistry
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18442
_journal_page_last               18449
_journal_paper_doi               10.1039/D3NJ03729K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C44 H35 Fe N2 O3 P Pt, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C44 H35 Fe N2 O3 P Pt'
_chemical_formula_weight         921.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4792(10)
_cell_length_b                   11.2400(5)
_cell_length_c                   26.6119(12)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.43
_cell_volume                     7140.1(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.9'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2017)'
_computing_publication_material  'PLATON (Spek, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            46973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.568
_diffrn_reflns_theta_min         2.081
_exptl_absorpt_coefficient_mu    4.411
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       prism
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.000412(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+12.0491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7746
_reflns_number_total             8231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03729k2.cif
_cod_data_source_block           fh410_sq
_cod_depositor_comments
'Adding full bibliography for 7062733--7062734.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7062734
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.405
_shelx_estimated_absorpt_t_max   0.719
_shelx_res_checksum              69647
_shelx_fab_checksum              24796