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_4065343
_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 H63 N2 O4 P2 Rb'
_chemical_formula_sum            'C51 H63 N2 O4 P2 Rb'
_chemical_formula_weight         915.44
_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
;
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                100.160(3)
_cell_angle_beta                 91.234(3)
_cell_angle_gamma                93.885(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1549(4)
_cell_length_b                   12.6068(4)
_cell_length_c                   17.4105(6)
_cell_measurement_reflns_used    10091
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.47
_cell_measurement_theta_min      3.57
_cell_volume                     2403.07(14)
_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 0.969
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19522
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.64
_diffrn_reflns_theta_min         3.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 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            yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.4539
_exptl_crystal_size_mid          0.3447
_exptl_crystal_size_min          0.1504
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0466P)^2^+1.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                8750
_reflns_number_total             9539
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200729x_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        2403.05(15)
_cod_database_code               4065343