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_7704339
_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         'C76 H72 B2 N4 O2, 2(C H Cl3)'
_chemical_formula_sum            'C78 H74 B2 Cl6 N4 O2'
_chemical_formula_weight         1333.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-05
_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                90
_cell_angle_beta                 108.166(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.990(2)
_cell_length_b                   18.4811(17)
_cell_length_c                   17.3011(17)
_cell_measurement_reflns_used    3153
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.110
_cell_measurement_theta_min      2.717
_cell_volume                     7592.1(12)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.1419
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46270
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         1.396
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0938 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8194. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       needle
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7001
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3099
_reflns_number_total             7001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01024c2.cif
_cod_data_source_block           kv_te_cb_bme_0m
_cod_depositor_comments
'Adding full bibliography for 7704339--7704342.cif.'
_cod_original_cell_volume        7592.2(12)
_cod_database_code               7704339
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36-C37
 1.54 with sigma of 0.002
 C37-C36 = C37-C38B = C37-C38A
 1.54 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C38A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C33, C34, C35, C36, C37, C38B, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H39A(0.5) H39(0.5) H37A(0.65) H37B(0.65) H37C(0.35) H37D(0.35)
 C38B(0.65) H38A(0.65) H38B(0.65) H38C(0.65) C38A(0.35) H38D(0.35) H38E(0.35)
 H38F(0.35) Cl2B(0.5) Cl1B(0.5) Cl3B(0.5) Cl3A(0.5) Cl1A(0.5) Cl2A(0.5)
6.a Ternary CH refined with riding coordinates:
 C39(H39A), C39(H39)
6.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C33(H33A,H33B), C37(H37A,
 H37B), C37(H37C,H37D)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C23(H23), C24(H24), C30(H30), C26(H26), C13(H13),
 C12(H12), C21(H21), C20(H20), C19(H19), C18(H18), C17(H17), C7(H7), C6(H6),
 C5(H5), C4(H4)
6.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C38B(H38A,H38B,H38C), C38A(H38D,
 H38E,H38F)
;
_shelx_res_checksum              81085
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'