Synthesis and characterisation of p-block complexes of biquinoline at different ligand charge states.
Hurmalainen, Juha; Mansikkamäki, Akseli; Morgan, Ian S.; Peuronen, Anssi; Tuononen, Heikki M.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1377–1381; doi:10.1039/c6dt04504a

data_7041661
_publ_section_title
;
 Synthesis and characterisation of p-block complexes of biquinoline at
 different ligand charge states.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1377
_journal_page_last               1381
_journal_paper_doi               10.1039/c6dt04504a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C18 H12 B Cl2 N2'
_chemical_formula_sum            'C18 H12 B Cl2 N2'
_chemical_formula_weight         338.01
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2016-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-23 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                86.739(15)
_cell_angle_beta                 86.016(15)
_cell_angle_gamma                86.206(15)
_cell_formula_units_Z            2
_cell_length_a                   6.7519(13)
_cell_length_b                   7.7698(14)
_cell_length_c                   14.179(3)
_cell_measurement_reflns_used    1604
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.3910
_cell_measurement_theta_min      5.6970
_cell_volume                     739.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega -110.00  -22.00   2.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -57.0000  150.0000 44

  2 omega  -69.00   29.00   2.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   57.0000  -60.0000 49

  3 omega  -23.00   73.00   2.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176  -77.0000   30.0000 48

  4 omega   33.00  121.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688 -125.0000  -30.0000 44

  5 omega   27.00   97.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -94.0000 -180.0000 35

  6 omega   25.00  107.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -94.0000    0.0000 41

  7 omega   42.00  104.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -94.0000   90.0000 31

  8 omega   90.00  166.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688   45.0000  150.0000 38

  9 omega   91.00  175.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688   45.0000   90.0000 42

 10 omega   94.00  164.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  125.0000    0.0000 35

 11 omega   46.00   90.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -30.0000  120.0000 22

 12 omega   69.00   97.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -45.0000 -120.0000 14

 13 omega   66.00   98.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -45.0000   30.0000 16

 14 omega   30.00   90.00   2.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5688  -30.0000  -30.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0198412000
_diffrn_orient_matrix_UB_12      0.1859425000
_diffrn_orient_matrix_UB_13      -0.0417782000
_diffrn_orient_matrix_UB_21      0.1803831000
_diffrn_orient_matrix_UB_22      0.0171053000
_diffrn_orient_matrix_UB_23      0.0588784000
_diffrn_orient_matrix_UB_31      0.1399490000
_diffrn_orient_matrix_UB_32      -0.0687620000
_diffrn_orient_matrix_UB_33      -0.0817471000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4291
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.998
_diffrn_reflns_theta_min         5.715
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       needle
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.1276
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.0194
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0985P)^2^+0.1434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2150
_reflns_number_total             2698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04504a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7041660--7041661.cif.'
_cod_original_cell_volume        739.4(2)
_cod_database_code               7041661
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C18 H12 N2 B1 Cl2'
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'