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_4111065
_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            'C31 H38 Ca N2 P2 Si2'
_chemical_formula_weight         596.83
_chemical_name_common            bis(iminophosphorano)methandiide-Calcium
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.7440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.2067(5)
_cell_length_b                   12.2438(3)
_cell_length_c                   27.0581(5)
_cell_measurement_temperature    203(2)
_cell_volume                     6740.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41184
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.374
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0502P)^2^+3.4321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                4941
_reflns_number_total             6866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065000zsi20060720_112526_2.cif
_cod_data_source_block           hasj17
_cod_database_code               4111065