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_4328060
_publ_contact_author_address
;Advanced Materials 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            'C31 H78 Mg2 N3 P3 Si3'
_chemical_formula_weight         718.76
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8848(5)
_cell_length_b                   18.5826(9)
_cell_length_c                   20.5032(9)
_cell_measurement_reflns_used    9293
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.26
_cell_volume                     4528.1(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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            105886
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9254
_exptl_absorpt_correction_T_min  0.8745
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_description       chip
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         11234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0465P)^2^+1.2751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                9946
_reflns_number_total             11234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202399z_si_004.cif
_cod_data_source_block           rkdd123_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4328060