Novel organocycloborates via Grignard reagentsElectronic supplementary information (ESI) available: experimental details and 1H, 13C and 11B NMR data for 1, 2, 3and 4, single crystal X-ray data and additional figures for 3and 4. See http://www.rsc.org/suppdata/cc/b4/b404864d/
Braunschweig, Holger; D'Andola, Giovanni; Welton, Tom; White, Andrew J. P.; Chemical Communications  (2004) 1738–1739; doi:10.1039/b404864d

data_7110321
_publ_section_title
;
 Novel organocycloborates via Grignard reagentsElectronic supplementary
 information (ESI) available: experimental details and 1H, 13C and 11B NMR
 data for 1, 2, 3and 4, single crystal X-ray data and additional figures
 for 3and 4. See http://www.rsc.org/suppdata/cc/b4/b404864d/
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1738
_journal_page_last               1739
_journal_paper_doi               10.1039/b404864d
_journal_year                    2004
_chemical_formula_sum            'C37 H72 B Br Mg O6'
_chemical_formula_weight         727.98
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.597(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.953(2)
_cell_length_b                   14.4213(16)
_cell_length_c                   25.584(3)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.57
_cell_volume                     4033.2(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7435
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.8712
_exptl_absorpt_correction_T_min  0.5761
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7040
_refine_ls_number_restraints     626
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                4555
_reflns_number_total             7040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b404864dsup1.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4033.4(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110321