Boratriazines: inducing luminescence through boron incorporation into a terpy-type framework
Yousaf, Muhammad; Yutronkie, Nathan J.; Castañeda, Raúl; Klein, Jacob A.; Brusso, Jaclyn; New J. Chem.  (2017) –; doi:10.1039/C7NJ02462B

data_7056617
_publ_section_title
;
 Boratriazines: inducing luminescence through boron incorporation into a
 terpy-type framework
;
_journal_name_full               'New J. Chem.'
_journal_paper_doi               10.1039/C7NJ02462B
_journal_year                    2017
_chemical_formula_moiety         'C H2 Cl2, C10 H8 B F2 N7'
_chemical_formula_sum            'C11 H10 B Cl2 F2 N7'
_chemical_formula_weight         359.97
_chemical_name_systematic
2,2-difluoro-4,6-bis(2-pyrimidyl)-1,3-dihydro-1,3,5,2-triazaborinine
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7915(7)
_cell_length_b                   10.7841(8)
_cell_length_c                   28.665(2)
_cell_measurement_reflns_used    2945
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.52
_cell_volume                     3026.8(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13127
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0980 before and 0.0614 after correction. The Ratio of minimum to maximum transmission is 0.7537. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2913
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0831P)^2^+3.4864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1794
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1709
_reflns_number_total             2913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02462b2.cif
_cod_data_source_block           F2PmBTA
_cod_original_cell_volume        3026.9(4)
_cod_database_code               7056617
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All N(H) groups
2. Restrained distances
 Cl1A-C11 \\sim Cl2-C11 \\sim Cl2A-C11 \\sim Cl1-C11
 with sigma of 0.02
 N5-H5 \\sim N3-H3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Cl2A) = Uanis(Cl1A) = Uanis(Cl1)
4. Others
 Sof(H11C)=Sof(H11D)=Sof(Cl2A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(H11A)=Sof(H11B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11(H11C,H11D)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C2(H2), C8(H8), C3(H3A), C1(H1)
;
_shelx_res_checksum              79080
_olex2_submission_special_instructions 'No special instructions were received'