Synthesis of borasiloxane-based macrocycles by multicomponent condensation reactions in solution or in a ball mill
Mirela Pascu; Albert Ruggi; Rosario Scopelliti; Kay Severin; Chem.Commun. 49 (2013) 45–; doi:10.1039/c2cc37538a

data_7108712
_publ_section_title
;
 Synthesis of borasiloxane-based macrocycles by multicomponent
 condensation reactions in solution or in a ball mill
;
_journal_name_full               Chem.Commun.
_journal_page_first              45
_journal_paper_doi               10.1039/c2cc37538a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C30 H46 B2 O6 Si2'
_chemical_formula_sum            'C30 H46 B2 O6 Si2'
_chemical_formula_weight         580.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-10-30 # Formatted by publCIF
;
_cell_angle_alpha                109.911(7)
_cell_angle_beta                 94.902(8)
_cell_angle_gamma                109.903(7)
_cell_formula_units_Z            1
_cell_length_a                   8.4713(9)
_cell_length_b                   10.5851(7)
_cell_length_c                   10.6720(11)
_cell_measurement_reflns_used    161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     823.76(15)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10453
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3753
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.4927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                2981
_reflns_number_total             3753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37538a.txt
_cod_data_source_block           mp016
_cod_original_cell_volume        823.76(13)
_cod_database_code               7108712