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_4075656
_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         'C74 H92 Ca2 N4'
_chemical_formula_sum            'C74 H92 Ca2 N4'
_chemical_formula_weight         1117.68
_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             2004-05-20T09:17:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.482(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0572(3)
_cell_length_b                   13.0076(3)
_cell_length_c                   17.5209(4)
_cell_measurement_reflns_used    13722
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     3374.34(13)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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      -0.121658E-1
_diffrn_orient_matrix_UB_12      -0.500961E-1
_diffrn_orient_matrix_UB_13      0.401527E-1
_diffrn_orient_matrix_UB_21      -0.602717E-1
_diffrn_orient_matrix_UB_22      -0.159031E-1
_diffrn_orient_matrix_UB_23      -0.323155E-1
_diffrn_orient_matrix_UB_31      0.279473E-1
_diffrn_orient_matrix_UB_32      -0.561045E-1
_diffrn_orient_matrix_UB_33      -0.266927E-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  0.0325
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23366
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.88
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_correction_T_min  0.8872
_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    1.1
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0465P)^2^+1.4476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                5121
_reflns_number_total             5859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0490334si20041208_044727.cif
_cod_data_source_block           may1704
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075656