B‒N coordinated triaryl pyrazole: effect of dimerization, and optical and NLO properties
Mukundam, Vanga; Sa, Shreenibasa; Kumari, Anupa; Das, Ritwick; Venkatasubbaiah, Krishnan; Journal of Materials Chemistry C 7 (2019) 12725–; doi:10.1039/C9TC04309H

data_7237991
_publ_section_title
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 B--N coordinated triaryl pyrazole: effect of dimerization, and optical
 and NLO properties
;
_journal_issue                   40
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              12725
_journal_paper_doi               10.1039/C9TC04309H
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C71 H72 B2 N4'
_chemical_formula_sum            'C71 H72 B2 N4'
_chemical_formula_weight         1002.94
_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   geom
_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
;
2019-06-25 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                109.303(4)
_cell_angle_beta                 95.233(4)
_cell_angle_gamma                112.832(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4091(6)
_cell_length_b                   14.0249(7)
_cell_length_c                   19.5464(13)
_cell_measurement_reflns_used    3371
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.71
_cell_measurement_theta_min      2.24
_cell_volume                     3094.0(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38403
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         1.141
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0711 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8944.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         11760
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0882P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6707
_reflns_number_total             11760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc04309h2.cif
_cod_data_source_block           mukund_pz_dimer_flu
_cod_database_code               7237991
_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. Rigid body (RIGU) restrains
 C66, C67, C68, C69A, C70A, C71A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, C67, C68, C69B, C70B, C71B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C70A(0.65) H70A(0.65) H70B(0.65) H68C(0.65) H68D(0.65) H68A(0.35)
 H68B(0.35) C69A(0.65) H69A(0.65) H69B(0.65) C71A(0.65) H71A(0.65) H71B(0.65)
 H71C(0.65) C70B(0.35) H70C(0.35) H70D(0.35) C71B(0.35) H71D(0.35) H71E(0.35)
 H71F(0.35) C69B(0.35) H69C(0.35) H69D(0.35)
4.a Secondary CH2 refined with riding coordinates:
 C70A(H70A,H70B), C66(H66A,H66B), C67(H67A,H67B), C68(H68C,H68D), C68(H68A,
 H68B), C69A(H69A,H69B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C70B(H70C,H70D), C69B(H69C,H69D)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C20(H20), C33(H33), C30(H30), C39(H39), C44(H44),
 C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C47(H47), C48(H48), C41(H41),
  C36(H36), C35(H35), C28(H28), C27(H27), C24(H24), C23(H23), C4AA(H4AA),
 C15(H15), C14(H14), C13(H13), C12(H12), C11(H11), C2AA(H2AA), C1AA(H1AA),
 C17(H17), C18(H18), C50(H50), C51(H51)
4.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C57(H57A,H57B,
 H57C), C56(H56A,H56B,H56C), C71A(H71A,H71B,H71C), C71B(H71D,H71E,H71F)
;
_shelx_res_checksum              48728
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'