Variable coordination of a chiral diphosphine containing an amidinium/NHC group within its backbone: μ-P,P', κ2-P,P' and κ3-P,C,P' coordination modes.
Newman, Paul D.; Cavell, Kingsley J.; Kariuki, Benson M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 12395–12407; doi:10.1039/c2dt31475d

data_7020412
_publ_section_title
;
 Variable coordination of a chiral diphosphine containing an amidinium/NHC
 group within its backbone: \m-P,P', \k2-P,P' and \k3-P,C,P' coordination
 modes.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12395
_journal_page_last               12407
_journal_paper_doi               10.1039/c2dt31475d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C94 H94 I4 N4 P4 Pd2, 0.27(I), 1.73(P F6) '
_chemical_formula_sum            'C94 H94 F10.4 I4.27 N4 P5.73 Pd2'
_chemical_formula_weight         2409.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.8377(9)
_cell_length_b                   19.8686(12)
_cell_length_c                   21.6459(13)
_cell_measurement_reflns_used    8498
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      1.19
_cell_volume                     11972.3(11)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD 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  0.1256
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31434
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.7494
_exptl_absorpt_correction_T_min  0.6567
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4735
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.294
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(5)
_refine_ls_extinction_coef       0.0030(3)
_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   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         12167
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2721
_refine_ls_wR_factor_ref         0.2961
_reflns_number_gt                8498
_reflns_number_total             12167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31475d.txt
_cod_data_source_block           kjc1139
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21212
_cod_original_formula_sum        'C94 H94 F10.40 I4.27 N4 P5.73 Pd2'
_cod_database_code               7020412