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_4073120
_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         'C20 H24 B N'
_chemical_formula_sum            'C20 H24 B N'
_chemical_formula_weight         289.21
_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             2007-05-03T12:01:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.252(1)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   10.1918(2)
_cell_length_b                   27.4592(5)
_cell_length_c                   18.0685(2)
_cell_measurement_reflns_used    31717
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     4990.84(15)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      0.982654E-1
_diffrn_orient_matrix_UB_12      -0.7333E-3
_diffrn_orient_matrix_UB_13      0.6068E-3
_diffrn_orient_matrix_UB_21      -0.145784E-1
_diffrn_orient_matrix_UB_22      0.43288E-2
_diffrn_orient_matrix_UB_23      -0.556719E-1
_diffrn_orient_matrix_UB_31      0.37389E-2
_diffrn_orient_matrix_UB_32      0.36152E-1
_diffrn_orient_matrix_UB_33      0.66784E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43181
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+2.0215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                6871
_reflns_number_total             9760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070083t-file004.cif
_cod_data_source_block           may407
_cod_original_cell_volume        4990.84(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4073120