Tris(imidazolin-2-ylidene-1-yl)borate Complexes of the Heavier Alkaline Earths: Synthesis and Structural Studies
Arrowsmith, Merle; Heath, Alex; Hill, Michael S.; Hitchcock, Peter B.; Kociok-Köhn, Gabriele; Organometallics 28 (2009) 4550–; doi:10.1021/om9003994

data_4069744
_publ_section_title
;
 Tris(imidazolin-2-ylidene-1-yl)borate Complexes of the Heavier Alkaline
 Earths: Synthesis and Structural Studies
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4550
_journal_paper_doi               10.1021/om9003994
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C25 H42 B Ca I N6 O), 3(C7 H8)'
_chemical_formula_sum            'C71 H108 B2 Ca2 I2 N12 O2'
_chemical_formula_weight         1517.27
_chemical_name_systematic
;
 ?
;
_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             2006-04-21T15:20:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.155(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.4848(16)
_cell_length_b                   10.5873(9)
_cell_length_c                   20.6304(15)
_cell_measurement_reflns_used    265572
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     4031.3(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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_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      -0.52493E-1
_diffrn_orient_matrix_UB_12      -0.16616E-2
_diffrn_orient_matrix_UB_13      -0.145616E-1
_diffrn_orient_matrix_UB_21      -0.13389E-1
_diffrn_orient_matrix_UB_22      0.3802E-3
_diffrn_orient_matrix_UB_23      0.463082E-1
_diffrn_orient_matrix_UB_31      -0.8697E-3
_diffrn_orient_matrix_UB_32      0.944374E-1
_diffrn_orient_matrix_UB_33      -0.4427E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24028
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.9141
_exptl_absorpt_correction_T_min  0.7156
_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    1.25
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7870
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0412P)^2^+10.8611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                5779
_reflns_number_total             7870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003994_si_002.cif
_cod_data_source_block           apr1706
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4069744