Synthesis and Characterization of a Sterically Encumbered Unsymmetrical 9-Borafluorene, Its Pyridine Adduct, and Its Dilithium Salt
Wehmschulte, Rudolf J.; Khan, Masood A.; Twamley, Brendan; Schiemenz, Berthold; Organometallics 20 (2001) 844–; doi:10.1021/om000868y

data_4077236
_publ_section_title
;
 Synthesis and Characterization of a Sterically Encumbered Unsymmetrical
 9-Borafluorene, Its Pyridine Adduct, and Its Dilithium Salt
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              844
_journal_paper_doi               10.1021/om000868y
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C60 H69 B N'
_chemical_formula_weight         814.97
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.477(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.364(2)
_cell_length_b                   28.684(5)
_cell_length_c                   11.869(2)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      4.16
_cell_volume                     5228.9(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.1448
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9651
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        5.3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.56
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9116
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.303
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.1556
_refine_ls_R_factor_obs          0.0902
_refine_ls_shift/esd_max         -0.042
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+5.4202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3368
_refine_ls_wR_factor_obs         0.2351
_reflns_number_observed          5482
_reflns_number_total             9182
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000868y.cif
_cod_data_source_block           rw003c_COMPOUND_1.py.1/2C6H14
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+5.4202P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+5.4202P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5228.9(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077236