Heteroleptic Phenylcalcium Derivatives via Metathesis Reactions of PhCa(thf)4I with Potassium Compounds
Gärtner, Martin; Görls, Helmar; Westerhausen, Matthias; Organometallics 26 (2007) 1077–; doi:10.1021/om061021q

data_4072773
_publ_section_title
;
 Heteroleptic Phenylcalcium Derivatives via Metathesis Reactions of
 PhCa(thf)4I with Potassium Compounds
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1077
_journal_paper_doi               10.1021/om061021q
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C36 H51 Ca O4.5 P'
_chemical_formula_weight         626.82
_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                87.823(1)
_cell_angle_beta                 88.844(1)
_cell_angle_gamma                86.701(1)
_cell_formula_units_Z            4
_cell_length_a                   11.1262(2)
_cell_length_b                   12.4878(2)
_cell_length_c                   27.3473(5)
_cell_measurement_temperature    183(2)
_cell_volume                     3790.03(11)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            26442
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  1.0112
_exptl_absorpt_correction_T_min  0.9515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         16518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1609P)^2^+8.9902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2845
_refine_ls_wR_factor_ref         0.3188
_reflns_number_gt                11297
_reflns_number_total             16518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061021qsi20061107_022228.cif
_cod_data_source_block           FO2838
_cod_original_cell_volume        3790.0(1)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C36 H51 Ca O4.50 P'
_cod_database_code               4072773