Syntheses of rod-shaped fluorescent 1,3,2-benzodiazaboroles with phosphonium, and phosphane chalcogenide acceptor functions.
Weber, Lothar; Kuhtz, Henry; Böhling, Lena; Brockhinke, Andreas; Chrostowska, Anna; Dargelos, Alain; Mazière, Audrey; Stammler, Hans-Georg; Neumann, Beate; Dalton transactions (Cambridge, England : 2003) 41 (2012) 10440–10452; doi:10.1039/c2dt30666b

data_7030262
_publ_section_title
;
 Syntheses of rod-shaped fluorescent 1,3,2-benzodiazaboroles with
 phosphonium, and phosphane chalcogenide acceptor functions.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10440
_journal_page_last               10452
_journal_paper_doi               10.1039/c2dt30666b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C28 H28 Au B Cl N2 P, (C5 H12 squeezed)'
_chemical_formula_sum            'C33 H40 Au B Cl N2 P'
_chemical_formula_weight         738.87
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 128.270(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.195(7)
_cell_length_b                   9.7525(16)
_cell_length_c                   22.556(3)
_cell_measurement_reflns_used    169
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.667
_cell_measurement_theta_min      3.449
_cell_volume                     5733(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_data_reduction
'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26951
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    5.308
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_correction_T_min  0.5684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
Der Kristall enth\"alt stark fehlgeordnetes n-Pentan.
Da die so resultierende Restelektronendichte nicht sinnvoll verfeinert
werden konnte, wurde die SQUEEZE-Routine des Programms PLATON (Spek, 2008)
angewandt. Die angegebene Summenformel sowie die darauf basierenden Parameter
ber\"ucksichtigen aber das fehlgeordnete L\"osungsmittel.

Spek, A. L. (2008) PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands

;
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+9.5926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                5205
_reflns_number_total             6552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30666b.txt
_cod_data_source_block           compound6
_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_cell_volume        5733.0(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7030262