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_4075655
_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         'C76 H96 Ca2 N4'
_chemical_formula_sum            'C76 H96 Ca2 N4'
_chemical_formula_weight         1145.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2004-09-15T10:05:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.916(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9183(3)
_cell_length_b                   13.1452(2)
_cell_length_c                   18.3729(4)
_cell_measurement_reflns_used    26627
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     3497.25(12)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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      -0.441685E-1
_diffrn_orient_matrix_UB_12      -0.458962E-1
_diffrn_orient_matrix_UB_13      -0.34554E-1
_diffrn_orient_matrix_UB_21      -0.255848E-1
_diffrn_orient_matrix_UB_22      -0.229045E-1
_diffrn_orient_matrix_UB_23      0.428292E-1
_diffrn_orient_matrix_UB_31      -0.465151E-1
_diffrn_orient_matrix_UB_32      0.56179E-1
_diffrn_orient_matrix_UB_33      -0.107676E-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  0.0448
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43924
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.857
_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    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0480P)^2^+1.4844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                5147
_reflns_number_total             6160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0490334si20041208_044710.cif
_cod_data_source_block           sep1804
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075655