Supramolecular Templating Approach for the Solvent-Free Synthesis of Open-Framework Metal Oxalates.
Guo, Furong; Chen, Cheng; Wang, Kangcai; Zhang, Qinghua; Lin, Zhien; Inorganic chemistry 55 (2016) 7817–7819; doi:10.1021/acs.inorgchem.6b01341

data_4348556
_publ_section_title
;
 Supramolecular Templating Approach for the Solvent-Free Synthesis of
 Open-Framework Metal Oxalates.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7817
_journal_page_last               7819
_journal_paper_doi               10.1021/acs.inorgchem.6b01341
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C3 In O10 S, C6 H16 N2'
_chemical_formula_sum            'C9 H16 In N2 O10 S'
_chemical_formula_weight         459.12
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.0767(6)
_cell_length_b                   26.0767(6)
_cell_length_c                   8.9467(3)
_cell_measurement_reflns_used    4592
_cell_measurement_temperature    293.55(10)
_cell_measurement_theta_max      28.1040
_cell_measurement_theta_min      3.9390
_cell_volume                     6083.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.55(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -9.00   99.00   1.0000   18.8700
omega____ theta____ kappa____ phi______ frames
    -       25.2025   57.0000   30.0000 108

  2 omega  -67.00   46.00   1.0000   18.8700
omega____ theta____ kappa____ phi______ frames
    -      -26.1400   77.0000 -150.0000 113
;
_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      0.0009732000
_diffrn_orient_matrix_UB_12      -0.0269968000
_diffrn_orient_matrix_UB_13      -0.0089455000
_diffrn_orient_matrix_UB_21      0.0262825000
_diffrn_orient_matrix_UB_22      0.0001513000
_diffrn_orient_matrix_UB_23      0.0202847000
_diffrn_orient_matrix_UB_31      -0.0068937000
_diffrn_orient_matrix_UB_32      -0.0032451000
_diffrn_orient_matrix_UB_33      0.0761798000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9187
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61371
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+7.9271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2733
_reflns_number_total             3117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01341_si_006.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4348556
_reflns_odcompleteness_completeness 99.67
_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, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), N2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              78731
_shelx_hkl_checksum              42602
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'