Isolation of an Intermediate in the Catalytic Trimerization of Isocyanates by a Monomeric Calcium Carbene with Chelating Iminophosphorane Substituents
Orzechowski, Lars; Harder, Sjoerd; Organometallics 26 (2007) 2144–; doi:10.1021/om070023n

data_4073037
_publ_section_title
;
 Isolation of an Intermediate in the Catalytic Trimerization of
 Isocyanates by a Monomeric Calcium Carbene with Chelating
 Iminophosphorane Substituents
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2144
_journal_paper_doi               10.1021/om070023n
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C57 H70 Ca N2 O2 P2'
_chemical_formula_weight         917.17
_chemical_name_common            C(Ph2P=N-(2,6-iPr-C6H3))Ca.THF2
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.7870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2645(2)
_cell_length_b                   24.1967(6)
_cell_length_c                   19.0740(4)
_cell_measurement_temperature    203(2)
_cell_volume                     5049.09(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            210551
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.231
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1968
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         14655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0511P)^2^+2.0728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                11098
_reflns_number_total             14655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070023nsi20070109_093232.cif
_cod_data_source_block           hasj41
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4073037