Crystal structure of 3,3′,3″-((1E,1′E,1″E)-((nitrilotris(ethane-2,1-diyl))tris(azaneylylidene)) tris(methaneylylidene))tris(4-hydroxy-1-naphthaldehyde) monohydrate, C42H36N4O6·H2O
Shi, Qing; Zhang, Qi-Long; Xu, Hong; Huang, Ya-Li; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 773–775; doi:10.1515/ncrs-2021-0120

data_8104707
_publ_section_title
;
 Crystal structure of
 3,3&#x2032;,3&#x2033;-((1E,1&#x2032;E,1&#x2033;E)-((nitrilotris(ethane-2,1-diyl))tris(azaneylylidene))
 tris(methaneylylidene))tris(4-hydroxy-1-naphthaldehyde) monohydrate,
 C42H36N4O6&#x00B7;H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              773
_journal_page_last               775
_journal_paper_doi               10.1515/ncrs-2021-0120
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C42 H36 N4 O6, H2 O'
_chemical_formula_sum            'C42 H38 N4 O7'
_chemical_formula_weight         710.76
_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
_cell_angle_alpha                113.563(2)
_cell_angle_beta                 96.740(2)
_cell_angle_gamma                104.429(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8563(6)
_cell_length_b                   12.6263(6)
_cell_length_c                   13.4492(6)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      34.54
_cell_measurement_theta_min      2.49
_cell_volume                     1733.07(15)
_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      301.72
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47868
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.489
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0633P)^2^+0.3643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5360
_reflns_number_total             6780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0120_suppl.cif
_cod_data_source_block           a
_cod_database_code               8104707
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C35A-O3
 1.22 with sigma of 0.02
 C35-O3A
 1.22 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O1X) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C35A) = Uanis(C35)
Uanis(O1X) = Uanis(O1W)
4. Others
 Sof(C35A)=Sof(H35A)=Sof(O3A)=1-FVAR(1)
 Sof(O3)=Sof(C35)=Sof(H35)=FVAR(1)
 Sof(O1X)=Sof(H1XA)=Sof(H1XB)=1-FVAR(2)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(2)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O1X(H1XA,H1XB)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C26(H26A,H26B),
 C27(H27A,H27B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C1(H1A), C2(H2), C5(H5), C7(H7), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C25(H25), C29(H29), C30(H30),
  C32(H32), C33(H33), C37(H37), C40(H40), C41(H41), C42(H42), C35A(H35A),
 C35(H35)
;