Crystal structure of (Z)-N-(4-(4-(4-((4,5,6-trimethoxy-3-oxobenzofuran-2(3H)-ylidene)methyl)phenoxy)butoxy)phenyl)acetamide, C30H31NO8
Xu, Lian-Hua; Shi, Ju-Mei; Wang, Hua-Bin; Zhou, Ying; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 987–989; doi:10.1515/ncrs-2023-0313

data_8107619
_publ_section_title
;
 Crystal structure of
 (Z)-N-(4-(4-(4-((4,5,6-trimethoxy-3-oxobenzofuran-2(3H)-ylidene)methyl)phenoxy)butoxy)phenyl)acetamide,
 C30H31NO8
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              987
_journal_page_last               989
_journal_paper_doi               10.1515/ncrs-2023-0313
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C30 H31 N O8'
_chemical_formula_sum            'C30 H31 N O8'
_chemical_formula_weight         533.56
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                82.199(2)
_cell_angle_beta                 88.113(2)
_cell_angle_gamma                81.617(2)
_cell_formula_units_Z            2
_cell_length_a                   5.21720(10)
_cell_length_b                   9.2878(2)
_cell_length_c                   27.2825(5)
_cell_measurement_reflns_used    4967
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8400
_cell_measurement_theta_min      4.8930
_cell_volume                     1295.66(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -89.00 -57.00   0.50    0.50    --    0.00 -41.00  66.16   64
  2  \w     58.00  84.00   0.50    0.50    --    0.00  19.00  60.00   52
  3  \w    -10.00  31.00   0.50    0.50    --    0.00 -82.00 -60.00   82
  4  \w    -36.00  18.00   0.50    0.50    --    0.00 -41.00  66.16  108
  5  \w    -13.00  29.00   0.50    0.50    --    0.00 -77.00  30.00   84
  6  \w    -18.00  28.00   0.50    0.50    --    0.00  19.00  60.00   92
  7  \w     86.00 123.00   0.50    0.50    --   95.80  30.00 120.00   74
  8  \w     24.00  81.00   0.50    0.50    --   95.80 -61.00 120.00  114
  9  \w      6.00  31.00   0.50    0.50    --   95.80 -15.00 150.00   50
 10  \w     61.00 126.00   0.50    0.50    --   95.80 -82.00-150.00  130
 11  \w    120.00 146.00   0.50    0.50    --   95.80  82.00-120.00   52
 12  \w     17.00  76.00   0.50    0.50    --   95.80 -45.00-180.00  118
 13  \w     40.00 126.00   0.50    0.50    --   95.80 -82.00 120.00  172
 14  \w      7.00 112.00   0.50    0.50    --   95.80 -30.00 -90.00  210
 15  \w     22.00 113.00   0.50    0.50    --   95.80 -45.00 -30.00  182
 16  \w     64.00 125.00   0.50    0.50    --   95.80 -77.00 -30.00  122
 17  \w     74.00 100.00   0.50    0.50    --   95.80 -82.00  60.00   52
 18  \w     71.00 127.00   0.50    0.50    --   95.80 -82.00-180.00  112
 19  \w     79.00 105.00   0.50    0.50    --   95.80  30.00 150.00   52
 20  \w    117.00 163.00   0.50    0.50    --   95.80  30.00 150.00   92
 21  \w     75.00 111.00   0.50    0.50    --   95.80 -82.00 -90.00   72
 22  \w      8.00  61.00   0.50    0.50    --   95.80 -82.00 -90.00  106
 23  \w    130.00 183.00   0.50    0.50    --   95.80  30.00 120.00  106
 24  \w     44.00 119.00   0.50    0.50    --   95.80 -15.00 150.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1125865000
_diffrn_orient_matrix_UB_12      -0.1112194000
_diffrn_orient_matrix_UB_13      0.0388326000
_diffrn_orient_matrix_UB_21      -0.0390018000
_diffrn_orient_matrix_UB_22      -0.0944700000
_diffrn_orient_matrix_UB_23      -0.0406651000
_diffrn_orient_matrix_UB_31      0.2736922000
_diffrn_orient_matrix_UB_32      -0.0855437000
_diffrn_orient_matrix_UB_33      0.0093456000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11979
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.257
_diffrn_reflns_theta_min         3.270
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0398P)^2^+1.9877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3886
_reflns_number_total             5027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0313_suppl_001.cif
_cod_data_source_block           62758
_cod_database_code               8107619
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C21(H21),
 C22(H22), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              99129
_shelx_hkl_checksum              21220
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.702