Synthesis of phosphinoferrocene amides and thioamides from carbamoyl chlorides and the structural chemistry of Group 11 metal complexes with these mixed-donor ligands.
Fernandes, Tiago A.; Solařová, Hana; Císařová, Ivana; Uhlík, Filip; Štícha, Martin; Štěpnička, Petr; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3092–3108; doi:10.1039/c4dt03279a

data_7033474
_publ_section_title
;
 Synthesis of phosphinoferrocene amides and thioamides from carbamoyl
 chlorides and the structural chemistry of Group 11 metal complexes with
 these mixed-donor ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3092
_journal_page_last               3108
_journal_paper_doi               10.1039/c4dt03279a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C50 H48 Ag2 Cl2 Fe2 N2 O8 P2 S2'
_chemical_formula_sum            'C50 H48 Ag2 Cl2 Fe2 N2 O8 P2 S2'
_chemical_formula_weight         1329.30
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-16 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0751(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9090(2)
_cell_length_b                   16.0180(5)
_cell_length_c                   19.5538(6)
_cell_measurement_reflns_used    5427
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      2.46
_cell_volume                     2452.64(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18097
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.632
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.374
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+14.8925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                4239
_reflns_number_total             5350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03279a2.cif
_cod_data_source_block           tfs
_cod_depositor_comments
'Adding full bibliography for 7033464--7033475.cif.'
_cod_database_code               7033474