Crystal structure of bis{1-phenyl-3-methyl-4-[(quinolin-3-yl)iminomethyl-κ<i>N</i>]-1<i>H</i>-pyrazol-5-olato-κ<i>O</i>}zinc methanol 2.5-solvate from synchrotron X-ray diffraction
Burlov, Anatoliy S.; Vlasenko, Valery G.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Khrustalev, Victor N.; Acta Crystallographica Section E 73 (2017) 1208–1212; doi:10.1107/S2056989017010441

data_2242115
_publ_section_title
;
 Crystal structure of
 bis{1-phenyl-3-methyl-4-[(quinolin-3-yl)iminomethyl-\k<i>N</i>]-1<i>H</i>-pyrazol-5-olato-\k<i>O</i>}zinc
 methanol 2.5-solvate from synchrotron X-ray diffraction
;
_journal_coeditor_code           WM5401
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1208
_journal_page_last               1212
_journal_paper_doi               10.1107/S2056989017010441
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Zn (C20 H15 N4 O1)2], 2.5C H4 O'
_chemical_formula_moiety         'C40 H30 N8 O2 Zn, 2.5(C H4 O)'
_chemical_formula_sum            'C44.5 H40 N8 O4.5 Zn'
_chemical_formula_weight         800.20
_chemical_name_systematic
'Bis{1-phenyl-3-methyl-4-[(quinolin-3-yl)iminomethyl-\k<i>N</i>]-1<i>H</i>-pyrazol-5-olato-\k<i>O</i>}zinc methanol 2.5-solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                111.56(3)
_cell_angle_beta                 114.71(3)
_cell_angle_gamma                96.30(3)
_cell_formula_units_Z            4
_cell_length_a                   15.569(3)
_cell_length_b                   16.994(3)
_cell_length_c                   17.035(3)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0
_cell_measurement_theta_min      3.3
_cell_volume                     3618(2)
_computing_cell_refinement
;
iMosflm (Battye <i>et al.</i>,  2011)
;
_computing_data_collection
;
Marccd (Doyle, 2011)
;
_computing_data_reduction
;
iMosflm (Battye <i>et al.</i>,  2011)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48608
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         41.445
_diffrn_reflns_theta_min         3.307
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SCALA</i>; Evans, 2006)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.028
_refine_diff_density_min         -1.002
_refine_ls_extinction_coef       0.0043(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         15616
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                12285
_reflns_number_total             15616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5401sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3618.1(16)
_cod_database_code               2242115
_shelx_estimated_absorpt_t_min   0.731
_shelx_estimated_absorpt_t_max   0.892
_shelx_hkl_checksum              7631
_shelx_res_checksum              39837
_shelxl_version_number           2014/6
_cod_database_fobs_code 2242115