New group 10 complexes of the bulky iminophosphine ligands [Ph2PCH2C(Ph)?N(2,6-R2C6H3)], where R = Me, iPr
Sofia I. Pascu; Karl S. Coleman; A. R. Cowley; Malcolm L. H. Green; Nicholas H. Rees; New Journal of Chemistry 29 (2005) 385–; doi:10.1039/b412391c

data_7050037
_publ_section_title
;
 New group 10 complexes of the bulky iminophosphine ligands
 [Ph2PCH2C(Ph)?N(2,6-R2C6H3)], where R = Me, iPr
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              385
_journal_paper_doi               10.1039/b412391c
_journal_volume                  29
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C40 H37 Br2 N Ni O P2, C1.24 H2.47 Cl2.47 '
_chemical_formula_sum            'C41.24 H39.47 Br2 Cl2.47 N Ni O P2'
_chemical_formula_weight         933.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5350(6)
_cell_length_b                   23.464(2)
_cell_length_c                   27.850(3)
_cell_measurement_reflns_used    49653
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     8844.7(13)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
Xpress Data collection (MAC Science, 1989)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type
;
Nonius DIP2000
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            49653
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         1.700
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.498
_exptl_absorpt_correction_T_max  0.536
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             3775.3
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.05
_refine_diff_density_min         -1.16
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2474
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         3915
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.008007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.64 0.420 1.28
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0962
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0658
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                3915
_reflns_number_total             8500
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b412391c.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        8844.7(12)
_cod_original_sg_symbol_H-M      'P c a b '
_cod_original_formula_sum        ' C41.24 H39.47 Br2 Cl2.47 N Ni O P2  '
_cod_database_code               7050037