Formation of Phosphino-Substituted Isocyanate by Reaction of CO2 with Group 2 Complexes Based on the (Me3Si)(i-Pr2P)NH Ligand
Diane A. Dickie; Kevin B. Gislason; Richard A. Kemp; Inorganic Chemistry 51 (2012) 1162–1169; doi:10.1021/ic202399z

data_4328058
_publ_contact_author_address
;Advanced Material Laboratory
Sandia National Laboratories
1001 University Blvd SE
Albuquerque, NM, 87106
USA
;
_publ_contact_author_email       rakemp@unm.edu
_publ_contact_author_name        'Kemp, Richard A.'
_publ_contact_author_phone       1-505-272-7609
_publ_section_title
;
 Formation of Phosphino-Substituted Isocyanate by Reaction of CO2 with
 Group 2 Complexes Based on the (Me3Si)(i-Pr2P)NH Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1162
_journal_page_last               1169
_journal_paper_doi               10.1021/ic202399z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C26 H62 Ca N2 O2 P2 Si2'
_chemical_formula_weight         592.98
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.947(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.4397(6)
_cell_length_b                   20.1683(6)
_cell_length_c                   20.6361(6)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.33
_cell_volume                     7335.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            152151
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.9185
_exptl_absorpt_correction_T_min  0.8447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         19746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+2.7905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                13305
_reflns_number_total             19746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202399z_si_002.cif
_cod_data_source_block           rkdd53m
_cod_database_code               4328058