Syntheses and Structure of the Solvent-Separated Calcium Cuprate [(thf)3Ca(μ-Ph)3Ca(thf)3]+[Ph−Cu−Ph]-
Fischer, Reinald; Görls, Helmar; Westerhausen, Matthias; Organometallics 26 (2007) 3269–; doi:10.1021/om700353w

data_4073473
_publ_section_title
;
 Syntheses and Structure of the Solvent-Separated Calcium Cuprate
 [(thf)3Ca(\m-Ph)3Ca(thf)3]+[Ph&#x2212;Cu&#x2212;Ph]-
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3269
_journal_paper_doi               10.1021/om700353w
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C54 H73 Ca2 Cu O6'
_chemical_formula_weight         961.82
_chemical_name_systematic
; 
 ? 
;
_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                 91.917(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5330(7)
_cell_length_b                   11.2561(4)
_cell_length_c                   20.6374(6)
_cell_measurement_temperature    183(2)
_cell_volume                     5231.4(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18399
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.9198
_exptl_absorpt_correction_T_min  0.8898
_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    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+3.9124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                3943
_reflns_number_total             6000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700353w-file002.cif
_cod_data_source_block           FO2828
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4073473