Synthesis, Structure, and Reactivity of a Stabilized Calcium Carbene: R2CCa
Lars Orzechowski; Georg Jansen; Sjoerd Harder; Journal of the American Chemical Society 128 (2006) 14676–14684; doi:10.1021/ja065000z

data_4111067
_publ_section_title
;
 Synthesis, Structure, and Reactivity of a Stabilized Calcium Carbene:
 R2CCa
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14676
_journal_page_last               14684
_journal_paper_doi               10.1021/ja065000z
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C81 H92 Ca2 N4 O P4 Si4'
_chemical_formula_weight         1453.99
_chemical_name_common
;
bis(iminophosphorano)methandiide-Calcium.(benzophenone)
;
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.391(2)
_cell_angle_beta                 92.101(2)
_cell_angle_gamma                102.574(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0694(4)
_cell_length_b                   16.2726(5)
_cell_length_c                   20.5634(7)
_cell_measurement_temperature    203(2)
_cell_volume                     4591.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            158090
_diffrn_reflns_theta_full        23.70
_diffrn_reflns_theta_max         23.70
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.286
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         13878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0558P)^2^+1.9857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                11701
_reflns_number_total             13878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065000zsi20060720_112526_4.cif
_cod_data_source_block           hasj27
_cod_original_cell_volume        4591.4(2)
_cod_database_code               4111067