Crystal structure of N′,N′′′-((1E,1′E)-(propane-2,2-diylbis(1H-pyrrole-5,2diyl))bis(methaneylylidene))di(nicotinohydrazide) pentahydrate, C25H24N8O2·5H2O
Zhou, Yi; Zhang, Min; Xiong, Ying; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1011–1013; doi:10.1515/ncrs-2021-0193

data_8104652
_publ_section_title
;
 Crystal structure of
 N&#x2032;,N&#x2032;&#x2032;&#x2032;-((1E,1&#x2032;E)-(propane-2,2-diylbis(1H-pyrrole-5,2diyl))bis(methaneylylidene))di(nicotinohydrazide)
 pentahydrate, C25H24N8O2&#x00B7;5H2O
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1011
_journal_page_last               1013
_journal_paper_doi               10.1515/ncrs-2021-0193
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C25 H24 N8 O2, 5(H2 O)'
_chemical_formula_sum            'C25 H34 N8 O7'
_chemical_formula_weight         558.60
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                93.062(8)
_cell_angle_beta                 97.015(9)
_cell_angle_gamma                99.478(8)
_cell_formula_units_Z            2
_cell_length_a                   7.507(2)
_cell_length_b                   8.0276(18)
_cell_length_c                   23.653(6)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.61
_cell_volume                     1391.5(6)
_computing_cell_refinement       'SAINT (Brucker, 2012)[2]'
_computing_data_collection       'APEX2 (Brucker, 2012)[2]'
_computing_data_reduction        'SAINT (Brucker, 2012)[2]'
_computing_molecular_graphics    'Diamond 4.0[4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[1]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.352
_diffrn_reflns_theta_min         2.580
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0789P)^2^+0.3341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5591
_reflns_number_total             6902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0193_suppl.cif
_cod_data_source_block           a
_cod_original_cell_volume        1391.4(6)
_cod_database_code               8104652
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O5W-H5WB
 0.86 with sigma of 0.02
 O5W-H5WA
 0.86 with sigma of 0.02
 O4W-H4WB
 0.86 with sigma of 0.02
 O4W-H4WA
 0.86 with sigma of 0.02
 O3W-H3WA
 0.86 with sigma of 0.02
 O3W-H3WB
 0.86 with sigma of 0.02
 O2W-H2WB
 0.86 with sigma of 0.02
 O2W-H2WA
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1WA) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1W) = Uanis(O1WA)
4. Others
 Sof(O1WA)=Sof(H1WC)=Sof(H1WD)=1-FVAR(1)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(1)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O1WA(H1WC,H1WD)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N5(H5), N7(H7), C1(H1), C2(H2A), C3(H3), C5(H5A), C7(H7A),
 C9(H9), C10(H10), C16(H16), C17(H17), C19(H19), C22(H22), C23(H23), C24(H24),
 C25(H25)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;