The synthesis and structure revision of NSC-134754
Jennie A. Hickin; Afshan Ahmed; Katharina Fuck; Margaret Ashcroft; Keith Jones; Chem.Commun. 50 (2014) 1238–; doi:10.1039/c3cc48189a

data_7111808
_publ_section_title
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 The synthesis and structure revision of NSC-134754
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_journal_name_full               Chem.Commun.
_journal_page_first              1238
_journal_paper_doi               10.1039/c3cc48189a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'O4 H S, 0.5(O4 S), C27 H36 N2 O2, H2 O'
_chemical_formula_sum            'C27 H39 N2 O9 S1.5'
_chemical_formula_weight         583.72
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-02-11
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.22(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.44(2)
_cell_length_b                   8.720(5)
_cell_length_c                   22.886(12)
_cell_measurement_temperature    120
_cell_volume                     5580(6)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.2076
_diffrn_reflns_av_unetI/netI     0.1975
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19949
_diffrn_reflns_theta_full        25.9996
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.9612
_exptl_absorpt_correction_T_min  0.9282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3897
_exptl_crystal_description       block
_exptl_crystal_F_000             2490.8596
_exptl_crystal_preparation       'soaked in perfluoro polyether oil'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.0669
_refine_diff_density_min         -1.0170
_refine_diff_density_rms         0.1354
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             8.3245
_refine_ls_goodness_of_fit_ref   0.9214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9214
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.0039
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              34
_reflns_limit_h_min              -38
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                2989
_reflns_number_total             5459
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c3cc48189a.txt
_cod_data_source_block           11srv156
_cod_database_code               7111808
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H6a,H6b} of C6, {H1a,H1b} of C1, {H19a,H19b} of C19, H9 of C9, H18 of C18,
  H24 of C24, H21 of C21, {H18a,H18b} of N18, {H14a,H14b} of C14, H1 of N1, H13
  of C13, H11 of C11, {H5a,H5b} of C5, {H2a,H2b} of C2, H17 of C17, {H4a,H4b}
  of C4, H10 of C10, {H16a,H16b} of C16
 At 1.5 times of:
  {H8a,H8b,H8c} of C8, {H26a,H26b,H26c} of C26, {H1Wa,H1Wb} of O1W, H3 of O3,
  {H27a,H27b,H27c} of C27
2. Others
 Fixed Sof: O7(0.5) O8(0.5) O3S(0.5)
3.a Ternary CH refined with riding coordinates:
 N1(H1), C17(H17)
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