The crystal structure of bis(2-acetyl-5-methoxyphenyl)carbonate 1.5 hydrate, C19H18O7
Liu, Juan; Chen, Sai; Li, Honglei; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1341–1343; doi:10.1515/ncrs-2021-0336

data_8104602
_publ_section_title
;
 The crystal structure of bis(2-acetyl-5-methoxyphenyl)carbonate 1.5
 hydrate, C19H18O7
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1341
_journal_page_last               1343
_journal_paper_doi               10.1515/ncrs-2021-0336
_journal_volume                  236
_journal_year                    2021
_chemical_absolute_configuration .
_chemical_formula_moiety         'C19 H18 O7, 1.5(H2 O)'
_chemical_formula_sum            'C19 H21 O8.5'
_chemical_formula_weight         385.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.467(3)
_cell_length_b                   39.168(8)
_cell_length_c                   7.6005(16)
_cell_measurement_reflns_used    6015
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.386
_cell_measurement_theta_min      2.259
_cell_volume                     3711.4(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            23174
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         1.040
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. 
wR2(int) was 0.0628 before and 0.0474 after correction. 
The Ratio of minimum to maximum transmission is 0.8667. 
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.0(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0479P)^2^+0.3902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                6621
_reflns_number_total             8508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0336_suppl.cif
_cod_data_source_block           zz
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H42 O17'
_cod_original_formula_weight         770.71
_cod_original_formula_moiety         '2(C19 H18 O7), 3(H2 O)'
_cod_original_formula_units_Z            4
_cod_database_code               8104602
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.0(10)
 0.0(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O10-H10B = O10-H10A = O9-H9E = O9-H9D = O8-H8B = O8-H8A
 0.84 with sigma of 0.02
 H10A-H10B
 1.46 with sigma of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C7(H7), C3(H3), C12(H12), C24(H24), C26(H26), C16(H16), C35(H35),
 C4(H4), C30(H30), C37(H37), C14(H14)
4.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C1(H1A,H1B,H1C),
 C38(H38A,H38B,H38C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C31(H31A,H31B,
 H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'