Reduced 3,4'-bipyrazoles from a simple pyrazole precursor: synthetic sequence, molecular structures and supramolecular assembly.
Cuartas, Viviana; Insuasty, Braulio; Cobo, Justo; Glidewell, Christopher; Acta crystallographica. Section C, Structural chemistry 73 (2017) 784–790; doi:10.1107/S205322961701302X

data_2311921
_publ_section_title
;
 Reduced 3,4'-bipyrazoles from a simple pyrazole precursor: synthetic
 sequence, molecular structures and supramolecular assembly.
;
_journal_coeditor_code           SK3669
_journal_issue                   'Pt 10'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              784
_journal_page_last               790
_journal_paper_doi               10.1107/S205322961701302X
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C28 H27 N5 O'
_chemical_formula_moiety         'C28 H27 N5 O'
_chemical_formula_sum            'C28 H27 N5 O'
_chemical_formula_weight         449.55
_chemical_name_systematic
(3<i>RS</i>)-5'-[Benzyl(methyl)amino]-3'-methyl-1',5-diphenyl-3,4-dihydro-1'<i>H</i>,2<i>H</i>-[3,4'-bipyrazole]-2-carbaldehyde
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.711(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   21.572(13)
_cell_length_c                   9.550(5)
_cell_measurement_reflns_used    5340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.562
_cell_measurement_theta_min      2.350
_cell_volume                     2311(2)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection       'APEX3 (Bruker2016)'
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL-2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1994)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            55209
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.562
_diffrn_reflns_theta_min         2.350
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS-2016/2; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
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_refine_diff_density_min         -0.294
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0445P)^2^+1.0860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
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_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3669sup1.cif
_cod_data_source_block           III
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_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              95060
_shelx_res_checksum              3097
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