Syntheses, structures and reactions of a series of β-diketiminatoyttrium compounds
Wei, Xuehong; Cheng, Yanxiang; Hitchcock, Peter B.; Lappert, Michael F.; Dalton Transactions  (2008) 5235–5246; doi:10.1039/b806451b

data_7004385
_publ_section_title
;
 Syntheses, structures and reactions of a series of
 \b-diketiminatoyttrium compounds
;
_journal_issue                   38
_journal_name_full               'Dalton Transactions'
_journal_page_first              5235
_journal_page_last               5246
_journal_paper_doi               10.1039/b806451b
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C98 H134 Cl4 K2 N6 O2 Y2, 4(C4 H10 O)'
_chemical_formula_sum            'C114 H174 Cl4 K2 N6 O6 Y2'
_chemical_formula_weight         2122.41
_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             2003-11-17T16:47:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.257(1)
_cell_angle_beta                 73.489(1)
_cell_angle_gamma                81.903(1)
_cell_formula_units_Z            1
_cell_length_a                   12.9490(1)
_cell_length_b                   14.4721(2)
_cell_length_c                   17.0897(2)
_cell_measurement_reflns_used    31166
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2886.47(6)
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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      0.18076E-1
_diffrn_orient_matrix_UB_12      -0.723572E-1
_diffrn_orient_matrix_UB_13      0.159619E-1
_diffrn_orient_matrix_UB_21      -0.652745E-1
_diffrn_orient_matrix_UB_22      -0.101019E-1
_diffrn_orient_matrix_UB_23      -0.158043E-1
_diffrn_orient_matrix_UB_31      0.437773E-1
_diffrn_orient_matrix_UB_32      0.8084E-2
_diffrn_orient_matrix_UB_33      -0.602234E-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  0.0501
_diffrn_reflns_av_unetI/netI     0.0428
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46919
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.7649
_exptl_absorpt_correction_T_min  0.7121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0315P)^2^+4.1679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.095
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                8871
_reflns_number_total             10598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b806451b.txt
_cod_data_source_block           (9)-nov1403
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004385