beta-Diiminato ligand (L) transformations in reactions of KL with PI3 and I2 [L = {N(C6H3Pr(i)2-2,6)C(H)}2CPh].
Hitchcock, Peter B; Lappert, Michael F; Li, Gang; Protchenko, Andrey V; Chemical communications (Cambridge, England)  (2007) 846–848; doi:10.1039/b611260a

data_7101715
_publ_section_title
;
 beta-Diiminato ligand (L) transformations in reactions of KL with PI3
 and I2 [L = {N(C6H3Pr(i)2-2,6)C(H)}2CPh].
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              846
_journal_page_last               848
_journal_paper_doi               10.1039/b611260a
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C66 H81 I N4 P, I3'
_chemical_formula_sum            'C66 H81 I4 N4 P'
_chemical_formula_weight         1468.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-01-17T09:59:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                67.651(1)
_cell_angle_beta                 88.601(2)
_cell_angle_gamma                79.776(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4165(2)
_cell_length_b                   17.3501(5)
_cell_length_c                   19.9124(6)
_cell_measurement_reflns_used    51338
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3271.88(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.538484E-1
_diffrn_orient_matrix_UB_12      -0.282554E-1
_diffrn_orient_matrix_UB_13      0.413097E-1
_diffrn_orient_matrix_UB_21      0.744794E-1
_diffrn_orient_matrix_UB_22      -0.108588E-1
_diffrn_orient_matrix_UB_23      0.350876E-1
_diffrn_orient_matrix_UB_31      -0.330251E-1
_diffrn_orient_matrix_UB_32      0.556791E-1
_diffrn_orient_matrix_UB_33      0.41644E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48640
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.391
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         12860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+11.1539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                8372
_reflns_number_total             12860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B611260A.txt
_cod_data_source_block           (1)-jan705
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101715