The crystal structure of 3-((4-chloro-N-(2-methoxyethyl)benzamido)methyl)phenyl methanesulfonate, C18H20ClNO5S
Li, Yong; Wu, Yundeng; Wang, Jingjing; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1033–1036; doi:10.1515/ncrs-2022-0376

data_8107285
_publ_section_title
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 The crystal structure of
 3-((4-chloro-N-(2-methoxyethyl)benzamido)methyl)phenyl methanesulfonate,
 C18H20ClNO5S
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_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1033
_journal_page_last               1036
_journal_paper_doi               10.1515/ncrs-2022-0376
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C18 H20 Cl N O5 S'
_chemical_formula_sum            'C18 H20 Cl N O5 S'
_chemical_formula_weight         397.86
_chemical_name_systematic
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3-((4-chloro-N-(2-methoxyethyl)benzamido)methyl)phenyl methanesulfonate
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_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90.18(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.671(4)
_cell_length_b                   18.225(13)
_cell_length_c                   17.99(2)
_cell_measurement_reflns_used    9074
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      32.68
_cell_measurement_theta_min      2.51
_cell_volume                     1859(3)
_computing_cell_refinement       'Bruker SAINT[1]'
_computing_data_collection       'Bruker APEX2[1]'
_computing_data_reduction        'Bruker SAINT[1]'
_computing_molecular_graphics    Olex2[4]
_computing_publication_material  Olex2[4],PLATON[5-8],publCIF[9]
_computing_structure_refinement  ShelXL[3]
_computing_structure_solution    ShelXT[2]
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20055
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.744
_diffrn_reflns_theta_min         2.235
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.7093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.9500.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4235
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0335P)^2^+0.7203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3660
_reflns_number_total             4235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0376_suppl.cif
_cod_data_source_block           1
_cod_database_code               8107285
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.976
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C9 \\sim C8-C9A
 with sigma of 0.02
 C10-O2 \\sim C10A-O2A
 with sigma of 0.02
 O2-C9 \\sim O2A-C9A
 with sigma of 0.02
 C8-O2 \\sim C8-O2A
 with sigma of 0.04
 C10-C9 \\sim C10A-C9A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C8 \\sim O2 \\sim C9 \\sim C10 \\sim O2A \\sim C9A \\sim C10A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(O2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10D)=
 Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(O2)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8AA,H8AB), C8(H8BC,H8BD), C11(H11A,H11B), C9(H9A,H9B), C9A(H9AA,H9AB)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C17(H17)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
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_shelx_res_checksum              10919
_shelx_hkl_checksum              41002
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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