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_4065342
_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 H59 N2 Na O2 P2'
_chemical_formula_sum            'C51 H59 N2 Na O2 P2'
_chemical_formula_weight         816.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.076(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6126(11)
_cell_length_b                   17.3394(18)
_cell_length_c                   24.612(3)
_cell_measurement_reflns_used    7086
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.26
_cell_volume                     4494.5(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.075
_diffrn_reflns_av_sigmaI/netI    0.054
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32765
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/2; Sheldrick, 1996)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.54
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         7918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.080P)^2^+1.753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.136
_refine_ls_wR_factor_ref         0.146
_reflns_number_gt                6227
_reflns_number_total             7918
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200729x_si_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        4494.4(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4065342