Synthesis and crystal structure of 4,4′-di(4-pyridyl)-6,6′-di(tert-butyl)-2,2′-[propylenedioxybis(nitrilomethylidyne)]diphenol, C35H40N4O4
Mu, Hao-Ran; Wang, Ji-Fa; Bian, Ruo-Nan; Dong, Wen-Kui; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 643–644; doi:10.1515/ncrs-2019-0876

data_8105244
_publ_section_title
;
 Synthesis and crystal structure of
 4,4&#x2032;-di(4-pyridyl)-6,6&#x2032;-di(tert-butyl)-2,2&#x2032;-[propylenedioxybis(nitrilomethylidyne)]diphenol,
 C35H40N4O4
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              643
_journal_page_last               644
_journal_paper_doi               10.1515/ncrs-2019-0876
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C35 H40 N4 O4'
_chemical_formula_sum            'C35 H40 N4 O4'
_chemical_formula_weight         580.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 101.2260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1768(5)
_cell_length_b                   6.07340(10)
_cell_length_c                   18.0123(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      66.59
_cell_measurement_theta_min      3.09
_cell_volume                     3130.75(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18294
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.629
_diffrn_reflns_theta_max         66.629
_diffrn_reflns_theta_min         3.088
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.027
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0623P)^2^+1.0672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2482
_reflns_number_total             2709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0876_suppl.cif
_cod_data_source_block           1125
_cod_database_code               8105244
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H18a(0.5) H18b(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18a,H18b), C17(H17a,H17b)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C16(H16), C9(H9), C6(H6), C7(H7), C8(H8)
3.c Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C14(H14a,H14b,H14c), C13(H13a,H13b,H13c)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;