Synthesis of π-extended B ← N coordinated phenanthroimidazole dimers and their linear and nonlinear optical properties.
Vanga, Mukundam; Sa, Shreenibasa; Kumari, Anupa; Murali, Anna Chandrasekar; Nayak, Prakash; Das, Ritwick; Venkatasubbaiah, Krishnan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7737–7746; doi:10.1039/d0dt01024c

data_7704340
_publ_section_title
;
 Synthesis of \p-extended B \\leftarrow N coordinated phenanthroimidazole
 dimers and their linear and nonlinear optical properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7737
_journal_page_last               7746
_journal_paper_doi               10.1039/d0dt01024c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C83 H76 B2 N4'
_chemical_formula_sum            'C83 H76 B2 N4'
_chemical_formula_weight         1151.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-08-06 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                103.453(4)
_cell_angle_beta                 115.561(4)
_cell_angle_gamma                105.550(3)
_cell_formula_units_Z            2
_cell_length_a                   15.4087(5)
_cell_length_b                   16.2830(6)
_cell_length_c                   16.8471(8)
_cell_measurement_reflns_used    6822
_cell_measurement_temperature    293.6(2)
_cell_measurement_theta_max      70.1380
_cell_measurement_theta_min      4.3390
_cell_volume                     3365.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_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      air
_diffrn_ambient_temperature      293.6(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     85.00 118.00   0.50    8.00    --   97.23  45.00  60.00   66
  2  \w    119.00 148.00   0.50    8.00    --   97.23  45.00  60.00   58
  3  \w     89.00 155.00   0.50    8.00    --   97.23  45.00  30.00  132
  4  \w     93.00 176.00   0.50    8.00    --   97.23  30.00  90.00  166
  5  \w     84.00 172.00   0.50    8.00    --   97.23  45.00 150.00  176
  6  \w     85.00 166.00   0.50    8.00    --   97.23  61.00 120.00  162
  7  \w    -10.00  42.00   0.50    2.00    --    0.00  57.00 -30.00  104
  8  \w    -11.00  76.00   0.50    2.00    --    0.00  38.00 -90.00  174
  9  \w    141.00 172.00   0.50    8.00    --   97.23 125.00 -90.00   62
 10  \w      0.00  46.00   0.50    2.00    --    0.00  77.00  90.00   92
 11  \w    -75.00 -50.00   0.50    2.00    --    0.00 -38.00-120.00   50
 12  \w     24.00 108.00   0.50    8.00    --   97.23 -95.00-150.00  168
 13  \w     90.00 117.00   0.50    8.00    --   97.23-125.00-120.00   54
 14  \w     31.00  57.00   0.50    8.00    --   97.23-125.00-120.00   52
 15  \w     53.00 104.00   0.50    8.00    --   97.23 -95.00  30.00  102
 16  \w     32.00  59.00   0.50    8.00    --   97.23-125.00  60.00   54
 17  \w     76.00 122.00   0.50    8.00    --   97.23-125.00  60.00   92
 18  \w     35.00 108.00   0.50    8.00    --   97.23 -95.00  90.00  146
 19  \w     34.00  97.00   0.50    8.00    --   97.23 -95.00 -60.00  126
 20  \w    -56.00  23.00   0.50    2.00    --    0.00 -77.00 150.00  158
 21  \w    -99.00 -61.00   0.50    8.00    --  -86.25  45.00 -30.00   76
 22  \w    -50.00 -16.00   0.50    8.00    --  -86.25  61.00-150.00   68
 23  \w    -99.00 -72.00   0.50    8.00    --  -86.25  61.00-150.00   54
 24  \w     31.00 114.00   0.50    8.00    --   97.23 -61.00 150.00  166
 25  \w    -17.00  12.00   0.50    2.00    --    0.00 -38.00-120.00   58
 26  \w     19.00  99.00   0.50    8.00    --   97.23 -15.00-180.00  160
 27  \w     25.00  92.00   0.50    8.00    --   97.23 -77.00 -60.00  134
 28  \w     23.00  92.00   0.50    8.00    --   97.23 -45.00 -30.00  138
 29  \w     30.00  96.00   0.50    8.00    --   97.23 -77.00  90.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0708454000
_diffrn_orient_matrix_UB_12      0.0478271000
_diffrn_orient_matrix_UB_13      -0.0329192000
_diffrn_orient_matrix_UB_21      0.0973221000
_diffrn_orient_matrix_UB_22      0.0400672000
_diffrn_orient_matrix_UB_23      0.1025113000
_diffrn_orient_matrix_UB_31      0.0205428000
_diffrn_orient_matrix_UB_32      -0.0871620000
_diffrn_orient_matrix_UB_33      -0.0254717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33325
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_min         4.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9d (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         12279
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1516P)^2^+1.0681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2417
_refine_ls_wR_factor_ref         0.2715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7761
_reflns_number_total             12279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01024c2.cif
_cod_data_source_block           sample1
_cod_depositor_comments
'Adding full bibliography for 7704339--7704342.cif.'
_cod_database_code               7704340
_chemical_oxdiff_formula         'C85 H76 N4'
_diffrn_oxdiff_ac3_digest_frames
;
01f53c4c4b49d8989220ef9bdd2f50de3f03180a807
;
_diffrn_oxdiff_ac3_digest_hkl
;
01f228e01f4658ae3cbd1c05f1277eb3347fb4
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C68-C67 \\sim C74-C67 \\sim C69-C68 \\sim C75-C74 \\sim C69-C70 \\sim C76-C75
\\sim C71-C70 \\sim C76-C77
 \\sim C71-C72 \\sim C78-C77 \\sim C73-C72 \\sim C78-C79
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C76 \\sim C77 \\sim C78 \\sim C79 \\sim C70 \\sim C71 \\sim C72 \\sim C73:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C69(H69A,H69B), C76(H76A,H76B), C70(H70A,H70B), C72(H72A,
 H72B), C77(H77A,H77B), C78(H78A,H78B), C71(H71A,H71B)
4.b Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C79(H79A,H79B,H79C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              83924
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.231
_oxdiff_exptl_absorpt_empirical_full_min 0.485