Crystal structure of (1<i>S</i>,3<i>R</i>,8<i>R</i>,9<i>R</i>,10<i>S</i>)-2,4,6-tris(2,2-dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.0^1,3^]dodec-9-yl)cyclotriboroxane
Benharref, Ahmed; El Ammari, Lahcen; Saadi, Mohamed; Mazoir, Noureddine; Berraho, Moha; Acta Crystallographica Section E 71 (2015) 941–943; doi:10.1107/S2056989015013390

data_2240937
_publ_section_title
;
 Crystal structure of
 (1<i>S</i>,3<i>R</i>,8<i>R</i>,9<i>R</i>,10<i>S</i>)-2,4,6-tris(2,2-dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.0^1,3^]dodec-9-yl)cyclotriboroxane
;
_journal_coeditor_code           IS5406
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              941
_journal_page_last               943
_journal_paper_doi               10.1107/S2056989015013390
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C48 H75 B3 Cl6 O3'
_chemical_formula_moiety         'C48 H75 B3 Cl6 O3'
_chemical_formula_sum            'C48 H75 B3 Cl6 O3'
_chemical_formula_weight         945.21
_chemical_name_systematic
(1<i>S</i>,3<i>R</i>,8<i>R</i>,9<i>R</i>,10<i>S</i>)-2,4,6-Tris(2,2-dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.0^1,3^]dodec-9-yl)cyclotriboroxane
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8240(2)
_cell_length_b                   21.1340(4)
_cell_length_c                   26.6620(7)
_cell_measurement_reflns_used    10143
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.5
_cell_volume                     4972.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0370
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43691
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.528
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       box
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.206
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3616 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.021(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         10143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+1.8134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                9010
_reflns_number_total             10143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5406sup1.cif
_cod_data_source_block           I
_cod_database_code               2240937
_cod_database_fobs_code          2240937
_shelx_hkl_checksum              48255
_shelx_res_checksum              14975
_shelxl_version_number           .2013