Novel access to carbodiphosphoranes in the coordination sphere of group 10 metals: template synthesis and protonation of PCP pincer carbodiphosphorane complexes of C(dppm)(2).
Reitsamer, Christian; Stallinger, Silvia; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Obendorf, Dagmar; Peringer, Paul; Dalton transactions (Cambridge, England : 2003) 41 (2012) 3503–3514; doi:10.1039/c2dt11949h

data_7018400
_publ_section_title
;
 Novel access to carbodiphosphoranes in the coordination sphere of group
 10 metals: template synthesis and protonation of PCP pincer
 carbodiphosphorane complexes of C(dppm)(2).
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3503
_journal_page_last               3514
_journal_paper_doi               10.1039/c2dt11949h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C103 H90 Cl8 Ni3 P8'
_chemical_formula_weight         2035.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.4335(2)
_cell_length_b                   17.4335(2)
_cell_length_c                   31.0829(4)
_cell_measurement_reflns_used    116640
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.0
_cell_volume                     8181.28(17)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37849
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green-blue
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         13390
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+1.5001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                11955
_reflns_number_total             13390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11949h.txt
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      P31
_cod_database_code               7018400