Dimerization of β-Diketiminato Calcium Complexes through Dihapto-Acetylide Ligation
Avent, Anthony G.; Crimmin, Mark R.; Hill, Michael S.; Hitchcock, Peter B.; Organometallics 24 (2005) 1184–; doi:10.1021/om0490334

data_4075654
_publ_section_title
;
 Dimerization of \b-Diketiminato Calcium Complexes through
 Dihapto-Acetylide Ligation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1184
_journal_paper_doi               10.1021/om0490334
_journal_volume                  24
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '(C70 H100 Ca2 N4), 2(C7 H8)'
_chemical_formula_sum            'C84 H116 Ca2 N4'
_chemical_formula_weight         1261.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-04-08T08:10:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                89.254(1)
_cell_angle_beta                 72.703(1)
_cell_angle_gamma                71.976(1)
_cell_formula_units_Z            1
_cell_length_a                   11.9217(2)
_cell_length_b                   13.2905(2)
_cell_length_c                   13.4317(2)
_cell_measurement_reflns_used    19517
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1924.91(5)
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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      0.509792E-1
_diffrn_orient_matrix_UB_12      -0.679801E-1
_diffrn_orient_matrix_UB_13      -0.443984E-1
_diffrn_orient_matrix_UB_21      -0.239986E-1
_diffrn_orient_matrix_UB_22      0.32174E-1
_diffrn_orient_matrix_UB_23      -0.613891E-1
_diffrn_orient_matrix_UB_31      0.736493E-1
_diffrn_orient_matrix_UB_32      0.255336E-1
_diffrn_orient_matrix_UB_33      -0.196713E-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  0.0388
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30434
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.9532
_exptl_absorpt_correction_T_min  0.9004
_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    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.8589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                7795
_reflns_number_total             8687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0490334si20041208_044648.cif
_cod_data_source_block           apr1104
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075654