The protonation state governs the coordination of phosphinoferrocene guanidines
Ondrej, Barta; Cisarova, Ivana; Štěpnička, Petr; Dalton Transactions  (2021) –; doi:10.1039/D1DT02884G

data_7708421
_publ_section_title
;
 The protonation state governs the coordination of phosphinoferrocene
 guanidines
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02884G
_journal_year                    2021
_chemical_formula_moiety         'C36 H38 Br Fe N4 P Pd, C H Cl3'
_chemical_formula_sum            'C37 H39 Br Cl3 Fe N4 P Pd'
_chemical_formula_weight         919.20
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                88.8870(10)
_cell_angle_beta                 84.124(2)
_cell_angle_gamma                86.8110(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4217(5)
_cell_length_b                   12.2753(5)
_cell_length_c                   13.5820(6)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.26
_cell_volume                     1891.14(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo with PHOTON III'
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.259
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.629
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0349P)^2^+3.2403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8344
_reflns_number_total             8639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02884g2.cif
_cod_data_source_block           ob445
_cod_database_code               7708421
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.431
_shelx_estimated_absorpt_t_max   0.794
_shelx_res_checksum              52371
_shelx_hkl_checksum              70824