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_2311922
_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          'C30 H31 N5 O2 , 0.945C2 H6 O'
_chemical_formula_moiety         'C30 H31 N5 O2 , 0.945C2 H6 O'
_chemical_formula_sum            'C31.89 H36.67 N5 O2.95'
_chemical_formula_weight         537.13
_chemical_name_systematic
;(3<i>RS</i>)-2-acetyl-5'-[Benzyl(methyl)amino]- 5-(4-methoxyphenyl)-3'-methyl-1'-phenyl-3,4-dihydro-1'<i>H</i>,2<i>H</i>-[3,4'-bipyrazole]
ethanol 0.945-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.04(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.363(6)
_cell_length_b                   28.238(18)
_cell_length_c                   10.775(7)
_cell_measurement_reflns_used    6555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.638
_cell_measurement_theta_min      2.307
_cell_volume                     2827(3)
_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 0.995
_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  0.0474
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            65713
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.638
_diffrn_reflns_theta_min         2.307
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS-2016/2; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       plate
_exptl_crystal_F_000             1146.3
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0430P)^2^+1.4625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                5518
_reflns_number_total             6550
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3669sup1.cif
_cod_data_source_block           IV
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2311922
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              83799
_shelx_res_checksum              94980
_shelxl_version_number           2.014