Group 1 Bis(iminophosphorano)methanides, Part 1:N-Alkyl and Silyl Derivatives of the Sterically Demanding Methanes H2C(PPh2NR)2(R = Adamantyl and Trimethylsilyl)
Wooles, Ashley J.; Gregson, Matthew; Cooper, Oliver J.; Middleton-Gear, Amy; Mills, David P.; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Organometallics 30 (2011) 5314–; doi:10.1021/om200553s

data_4065075
_publ_section_title
;
 Group 1 Bis(iminophosphorano)methanides, Part 1:N-Alkyl and Silyl
 Derivatives of the Sterically Demanding Methanes H2C(PPh2NR)2(R =
 Adamantyl and Trimethylsilyl)
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5314
_journal_paper_doi               10.1021/om200553s
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C53 H67 N2 Na O2 P2'
_chemical_formula_sum            'C53 H67 N2 Na O2 P2'
_chemical_formula_weight         849.02
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.7572(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   29.1701(4)
_cell_length_b                   20.3182(3)
_cell_length_c                   23.9244(3)
_cell_measurement_reflns_used    29832
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.45
_cell_measurement_theta_min      3.21
_cell_volume                     13646.8(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_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_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.027
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63777
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.61
_diffrn_reflns_theta_min         3.54
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  1.863
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.725
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.38
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         27221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0379
_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^)+(0.049P)^2^+6.643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.102
_reflns_number_gt                23818
_reflns_number_total             27221
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200553s_si_001.cif
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_database_code               4065075