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_4065351
_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         'C51 H55 I2 N2 O2 P2 Pr, 3(C7 H8)'
_chemical_formula_sum            'C72 H79 I2 N2 O2 P2 Pr'
_chemical_formula_weight         1461.02
_chemical_name_systematic
; 
 ? 
;
_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, 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                85.157(2)
_cell_angle_beta                 76.840(2)
_cell_angle_gamma                87.327(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7745(17)
_cell_length_b                   15.235(2)
_cell_length_c                   17.276(2)
_cell_measurement_reflns_used    11637
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.516
_cell_measurement_theta_min      2.2405
_cell_volume                     3261.0(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; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer(Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.045
_diffrn_reflns_av_sigmaI/netI    0.076
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28741
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.52
_refine_diff_density_min         -1.47
_refine_diff_density_rms
;0.17 
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Consequence of SQUEEZE.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         14697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.136
_refine_ls_wR_factor_ref         0.141
_reflns_number_gt                11326
_reflns_number_total             14697
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200729x_si_001.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' 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_cell_volume        3260.9(8)
_cod_database_code               4065351