Mono- and polynuclear Ag(i) complexes of N-functionalized bis(diphenylphosphino)amine DPPA-type ligands: synthesis, solid-state structures and reactivity.
Ghisolfi, Alessio; Fliedel, Christophe; de Frémont, Pierre; Braunstein, Pierre; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5571–5586; doi:10.1039/c6dt04755f

data_7042575
_publ_section_title
;
 Mono- and polynuclear Ag(i) complexes of N-functionalized
 bis(diphenylphosphino)amine DPPA-type ligands: synthesis, solid-state
 structures and reactivity.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5571
_journal_page_last               5586
_journal_paper_doi               10.1039/c6dt04755f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C93 H81 Ag3 Cl2 N3 O3 P6, B F4, C H2 Cl2 '
_chemical_formula_sum            'C94 H83 Ag3 B Cl4 F4 N3 O3 P6'
_chemical_formula_weight         2040.67
_chemical_name_common            AG121
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-08-01 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.25800(10)
_cell_length_b                   34.9966(5)
_cell_length_c                   29.4055(4)
_cell_measurement_reflns_used    252205
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     10191.8(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'sir 92'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_sigmaI/netI    0.0952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            98194
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.7893
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4128
_exptl_crystal_recrystallization_method 'DCM - Pentane'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
;
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.00087(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         19790
_refine_ls_number_restraints     1024
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2433
_refine_ls_wR_factor_ref         0.2630
_reflns_number_gt                10979
_reflns_number_total             19790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04755f2.cif
_cod_data_source_block           compound_4c-DCM
_cod_depositor_comments
'Adding full bibliography for 7042575--7042581.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7042575