β-Diketiminato Calcium Acetylides: Synthesis, Solution Dimerization, and Catalytic Carbon−Carbon Bond Formation
Barrett, Anthony G. M.; Crimmin, Mark R.; Hill, Michael S.; Hitchcock, Peter B.; Lomas, Sarah L.; Mahon, Mary F.; Procopiou, Panayiotis A.; Suntharalingam, Kogularamanan; Organometallics 27 (2008) 6300–; doi:10.1021/om800738r

data_4072297
_publ_section_title
;
 \b-Diketiminato Calcium Acetylides: Synthesis, Solution Dimerization, and
 Catalytic Carbon&#x2212;Carbon Bond Formation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6300
_journal_paper_doi               10.1021/om800738r
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C49 H70 Ca N4 O, 0.5(C6 H14)'
_chemical_formula_sum            'C52 H77 Ca N4 O'
_chemical_formula_weight         814.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-11-10T11:32:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.186(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7318(1)
_cell_length_b                   18.3367(2)
_cell_length_c                   23.4138(3)
_cell_measurement_reflns_used    53680
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5023.40(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.674081E-1
_diffrn_orient_matrix_UB_12      0.76085E-2
_diffrn_orient_matrix_UB_13      -0.231063E-1
_diffrn_orient_matrix_UB_21      -0.522719E-1
_diffrn_orient_matrix_UB_22      0.150871E-1
_diffrn_orient_matrix_UB_23      -0.335688E-1
_diffrn_orient_matrix_UB_31      0.53181E-2
_diffrn_orient_matrix_UB_32      0.518517E-1
_diffrn_orient_matrix_UB_33      0.13158E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            74797
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9922
_exptl_absorpt_correction_T_min  0.8934
_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    1.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         9878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+2.3362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.121
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                7978
_reflns_number_total             9878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800738r_si_002.cif
_cod_data_source_block           nov706
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072297