The crystal structure of oxonium chlorido-ethylenediaminetetraactetotin(IV) hydrate, C10H17ClN2O10Sn
Fu, Zhihai; Chen, Bo; He, Aidang; Lv, Xia; Wei, Xin; Feng, Xiaojie; Huang, Chao; Xia, ChuanQin; Jin, Yongdong; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 941–942; doi:10.1515/ncrs-2017-0092

data_8106729
_publ_section_title
;
 The crystal structure of oxonium
 chlorido-ethylenediaminetetraactetotin(IV) hydrate, C10H17ClN2O10Sn
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              941
_journal_page_last               942
_journal_paper_doi               10.1515/ncrs-2017-0092
_journal_volume                  232
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H12 Cl N2 O8 Sn, H2 O, H3 O'
_chemical_formula_sum            'C10 H17 Cl N2 O10 Sn'
_chemical_formula_weight         479.39
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                101.340(5)
_cell_angle_beta                 99.624(5)
_cell_angle_gamma                91.279(4)
_cell_formula_units_Z            1
_cell_length_a                   6.6666(3)
_cell_length_b                   6.6892(4)
_cell_length_c                   8.8779(6)
_cell_measurement_reflns_used    2768
_cell_measurement_temperature    294.28(15)
_cell_measurement_theta_max      29.0810
_cell_measurement_theta_min      4.2120
_cell_volume                     382.09(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.28(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details
;
  1 omega  -21.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0031   19.0000   30.0000 110

  2 omega   -1.00   85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0031   57.0000   90.0000 86

  3 omega  -20.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0031  -99.0000  -30.0000 77

  4 omega  -51.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0031  -57.0000 -150.0000 87

  5 omega  -49.00   11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9406  -78.0000   79.0000 60

  6 omega  -47.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9406   78.0000 -155.0000 75

  7 omega   34.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0031 -178.0000  150.0000 58

  8 omega   -5.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0031   38.0000  -90.0000 93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0034520000
_diffrn_orient_matrix_UB_12      -0.0941545000
_diffrn_orient_matrix_UB_13      -0.0538640000
_diffrn_orient_matrix_UB_21      -0.0601484000
_diffrn_orient_matrix_UB_22      -0.0461874000
_diffrn_orient_matrix_UB_23      0.0439972000
_diffrn_orient_matrix_UB_31      -0.0897444000
_diffrn_orient_matrix_UB_32      0.0271271000
_diffrn_orient_matrix_UB_33      -0.0448632000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5137
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_description       plate
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 1368 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3181
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.857
_reflns_Friedel_fraction_max     0.665
_reflns_number_gt                3180
_reflns_number_total             3181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0092_suppl.cif
_cod_data_source_block           xcq-fzh-2
_cod_original_cell_volume        382.08(4)
_cod_database_code               8106729
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O9-H9D
 0.85 with sigma of 0.02
 O9-H9E
 0.85 with sigma of 0.02
3.a Free rotating group:
 O10(H10A,H10B)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C9(H9A,H9B)
;
_shelx_res_checksum              18621
_shelx_hkl_checksum              74093
_olex2_date_sample_data_collection 2016-12-26
_olex2_submission_special_instructions 'No special instructions were received'