Ylidene→Iminophosphine Coordination Complexes and Reversible Dissociation of Dichlorophosphetidines
Neil Burford; C. Adam Dyker; Andrew D. Phillips; Heather A. Spinney; Andreas Decken; Robert McDonald; Paul J. Ragogna; Arnold L. Rheingold; Inorganic Chemistry 43 (2004) 7502–7507; doi:10.1021/ic049333d

data_4312015
_publ_contact_author_address
;
Department of Chemistry
Dalhousie University
Halifax, Nova Scotia
B3H 4J3
;
_publ_contact_author_email       ' Neil.Burford@dal.ca '
_publ_contact_author_fax         ' 902-494-1310 '
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       ' 902-494-3190 '
_publ_section_title
;
 Ylidene\\rightarrowIminophosphine Coordination Complexes and Reversible
 Dissociation of Dichlorophosphetidines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7502
_journal_page_last               7507
_journal_paper_doi               10.1021/ic049333d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C29 H49 I N3 P'
_chemical_formula_weight         597.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                77.1770(10)
_cell_angle_beta                 80.7610(10)
_cell_angle_gamma                65.1590(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4383(5)
_cell_length_b                   9.5486(6)
_cell_length_c                   21.4547(14)
_cell_measurement_reflns_used    5195
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.322
_cell_measurement_theta_min      2.386
_cell_volume                     1525.19(17)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6132
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.9460
_exptl_absorpt_correction_T_min  0.7439
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+1.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                4626
_reflns_number_total             6132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049333dsi20040523_084845_4.cif
_cod_data_source_block           Mes*NP(Im)I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4312015