Reactions of β-Diketiminate-Stabilized Calcium Amides with 9-Borabicyclo[3.3.1]nonane (9-BBN)
Barrett, Anthony G. M.; Crimmin, Mark R.; Hill, Michael S.; Hitchcock, Peter B.; Procopiou, Panayiotis A.; Organometallics 26 (2007) 4076–; doi:10.1021/om070083t

data_4073119
_publ_section_title
;
 Reactions of \b-Diketiminate-Stabilized Calcium Amides with
 9-Borabicyclo[3.3.1]nonane (9-BBN)
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4076
_journal_paper_doi               10.1021/om070083t
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C41 H65 B Ca N2 O'
_chemical_formula_sum            'C41 H65 B Ca N2 O'
_chemical_formula_weight         652.84
_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      2.3
_audit_creation_date             2006-05-17T13:31:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.568(10)
_cell_angle_beta                 101.002(9)
_cell_angle_gamma                97.642(5)
_cell_formula_units_Z            4
_cell_length_a                   12.2271(17)
_cell_length_b                   18.577(3)
_cell_length_c                   18.876(2)
_cell_measurement_reflns_used    422544
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     4019.7(10)
_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 0.923
_diffrn_measured_fraction_theta_max 0.923
_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      -0.27046E-1
_diffrn_orient_matrix_UB_12      -0.128181E-1
_diffrn_orient_matrix_UB_13      0.430826E-1
_diffrn_orient_matrix_UB_21      0.518182E-1
_diffrn_orient_matrix_UB_22      -0.372741E-1
_diffrn_orient_matrix_UB_23      0.12074E-2
_diffrn_orient_matrix_UB_31      0.614377E-1
_diffrn_orient_matrix_UB_32      0.402865E-1
_diffrn_orient_matrix_UB_33      0.357619E-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  0.089
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30593
_diffrn_reflns_theta_full        23.02
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.941
_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    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.25
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         10365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+6.1387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                6682
_reflns_number_total             10365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070083t-file001.cif
_cod_data_source_block           may2006
_cod_original_cell_volume        4019.8(9)
_cod_database_code               4073119