Group 1 Bis(iminophosphorano)methanides, Part 2:N-Aryl Derivatives of the Sterically Demanding Methanes H2C(PPh2NR)2(R = 2,4,6-trimethylphenyl or 2,6-diisopropylphenyl)
Wooles, Ashley J.; Gregson, Matthew; Robinson, Sarah; Cooper, Oliver J.; Mills, David P.; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Organometallics 30 (2011) 5326–; doi:10.1021/om200729x

data_4065349
_publ_section_title
;
 Group 1 Bis(iminophosphorano)methanides, Part 2:N-Aryl Derivatives of the
 Sterically Demanding Methanes H2C(PPh2NR)2(R = 2,4,6-trimethylphenyl or
 2,6-diisopropylphenyl)
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5326
_journal_paper_doi               10.1021/om200729x
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C61 H79 Cs N2 O3 P2, C4 H10 O'
_chemical_formula_sum            'C65 H89 Cs N2 O4 P2'
_chemical_formula_weight         1157.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7463(7)
_cell_length_b                   20.3503(13)
_cell_length_c                   28.0299(18)
_cell_measurement_reflns_used    17343
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.15
_cell_volume                     6111.3(7)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            37530
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'COLUMN    '
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.938
_refine_diff_density_min         -2.536
_refine_diff_density_rms
;0.092 
PROBLEM: Short Intra H...H Contact H64A .. H63A .. 1.63 Ang.
RESPONSE: Apparent short H-H distances are due to the disorder models.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         14051
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0719P)^2^+14.0387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                11364
_reflns_number_total             14051
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200729x_si_001.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4065349