Cycloaddition reactions of (C6F5)2BN3 with dialkyl acetylenedicarboxylates.
Melen, Rebecca L.; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 5045–5048; doi:10.1039/c5dt00316d

data_7702021
_publ_section_title
;
 Cycloaddition reactions of (C6F5)2BN3 with dialkyl
 acetylenedicarboxylates.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5045
_journal_page_last               5048
_journal_paper_doi               10.1039/c5dt00316d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C40 H20 B2 F20 N6 O8'
_chemical_formula_sum            'C40 H20 B2 F20 N6 O8'
_chemical_formula_weight         1114.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-06 deposited with the CCDC.
2015-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.618(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7165(16)
_cell_length_b                   12.7361(19)
_cell_length_c                   32.695(5)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.52
_cell_volume                     4441.0(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.7
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9814
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            37996
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         1.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.8569.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.6664
_exptl_crystal_description       Block
_exptl_crystal_F_000             2226.1811
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.0299
_refine_diff_density_min         -0.8882
_refine_diff_density_rms         0.1596
_refine_ls_d_res_high            0.7731
_refine_ls_d_res_low             11.8599
_refine_ls_goodness_of_fit_ref   1.0187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     688
_refine_ls_number_reflns         9887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0187
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0660P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              -11
_reflns_number_gt                5150
_reflns_number_total             9887
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt00316d2.cif
_cod_data_source_block           RLM032_0m
_cod_original_cell_volume        4440.9(11)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7702021
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C95(H95a,H95b), C70(H70a,H70b), C92(H92a,H92b), C4(H4a,H4b)
2.b Idealised Me refined as rotating group:
 C93(H93a,H93b,H93c), C96(H96a,H96b,H96c), C5(H5a,H5b,H5c), C76(H76a,H76b,H76c)
;
_olex2_submission_special_instructions 'No special instructions were received'