Synthesis of a 1-boratabenzene-(2,3,4,5-tetramethylphosphole): towards a planar monophosphole.
Bélanger-Chabot, Guillaume; Rioux, Philippe; Maron, Laurent; Fontaine, Frédéric-Georges; Chemical communications (Cambridge, England) 46 (2010) 6816–6818; doi:10.1039/c0cc01999b

data_7112858
_publ_section_title
;
 Synthesis of a 1-boratabenzene-(2,3,4,5-tetramethylphosphole): towards a
 planar monophosphole.
;
_journal_issue                   36
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6816
_journal_page_last               6818
_journal_paper_doi               10.1039/c0cc01999b
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C19 H33 B Li N2 P'
_chemical_formula_weight         338.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.435(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.766(3)
_cell_length_b                   18.191(7)
_cell_length_c                   13.428(5)
_cell_measurement_reflns_used    820
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.82
_cell_measurement_theta_min      2.24
_cell_volume                     2131.6(14)
_computing_cell_refinement       'APEX 2 (Bruker, 2005b)'
_computing_data_collection       'APEX 2 (Bruker, 2005b)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD'
_diffrn_measurement_method       \w
_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  0.1355
_diffrn_reflns_av_sigmaI/netI    0.1013
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19893
_diffrn_reflns_theta_full        24.24
_diffrn_reflns_theta_max         24.24
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9960
_exptl_absorpt_correction_T_min  0.9819
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Bruker, 2005a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3440
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.7035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                1764
_reflns_number_total             3440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01999b.txt
_cod_data_source_block           gbc044
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7112858