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_4111068
_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            'C47 H58 Ca N3 O P2 Si2'
_chemical_formula_weight         839.16
_chemical_name_common
;
bis(iminophosphorano)methandiide-Calcium + Cy-N=C=O
;
_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                 91.418(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8153(4)
_cell_length_b                   17.5149(5)
_cell_length_c                   18.9903(5)
_cell_measurement_temperature    203(2)
_cell_volume                     4593.7(2)
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41876
_diffrn_reflns_theta_full        26.71
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.296
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             1788
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0508P)^2^+1.5110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                7107
_reflns_number_total             9711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065000zsi20060720_112526_5.cif
_cod_data_source_block           hasj31
_cod_database_code               4111068