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_4111064
_publ_contact_author             'Sjoerd Harder'
_publ_contact_author_email       sjoerd.harder@uni-essen.de
_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            'C65 H81 Ca N4 P4 Si4'
_chemical_formula_weight         1194.66
_chemical_name_common            bis[(TMS-imino-di-Ph-phosphorano)methyl]Calcium
_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                77.7910(10)
_cell_angle_beta                 87.5050(10)
_cell_angle_gamma                68.7850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9706(2)
_cell_length_b                   14.8783(3)
_cell_length_c                   21.3712(4)
_cell_measurement_temperature    183(2)
_cell_volume                     3465.78(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            209015
_diffrn_reflns_theta_full        34.79
_diffrn_reflns_theta_max         34.79
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.291
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         28072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0635P)^2^+0.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                20002
_reflns_number_total             28072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065000zsi20060720_112526_1.cif
_cod_data_source_block           hasj23
_cod_database_code               4111064