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_4348557
_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         '0.5(C8 H28 O30 Zn6), 2(O4 S), C6 H16 N2'
_chemical_formula_sum            'C10 H30 N2 O23 S2 Zn3'
_chemical_formula_weight         806.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-23
_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            4
_cell_length_a                   11.10580(11)
_cell_length_b                   16.34489(16)
_cell_length_c                   14.00636(14)
_cell_measurement_reflns_used    4289
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5440
_cell_measurement_theta_min      4.1590
_cell_volume                     2542.48(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    1.5500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000   30.0000 94

  2 omega   23.00   90.00   1.0000    1.5500
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -180.0000 67

  3 omega    1.00   75.00   1.0000    1.5500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000 -180.0000 74

  4 omega  -33.00   55.00   1.0000    1.5500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000  120.0000 88

  5 omega   41.00  126.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  120.0000 85

  6 omega   38.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

  7 omega   38.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

  8 omega   81.00  176.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

  9 omega   44.00  104.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 60
;
_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      0.0218105000
_diffrn_orient_matrix_UB_12      -0.0532824000
_diffrn_orient_matrix_UB_13      -0.0890881000
_diffrn_orient_matrix_UB_21      -0.1197557000
_diffrn_orient_matrix_UB_22      -0.0449125000
_diffrn_orient_matrix_UB_23      0.0181404000
_diffrn_orient_matrix_UB_31      -0.0664772000
_diffrn_orient_matrix_UB_32      0.0634583000
_diffrn_orient_matrix_UB_33      -0.0619411000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.000
_diffrn_reflns_theta_min         5.082
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    2.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00145(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0858P)^2^+2.4248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2213
_reflns_number_total             2348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01341_si_002.cif
_cod_data_source_block           1
_cod_database_code               4348557
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: HW4A(0.5) HW4B(0.5)
3.a Riding coordinates:
 OW1(HW1A,HW1B), OW2(HW2A,HW2B)
3.b Rotating group:
 OW3(HW3A,HW3B), OW4(HW4A,HW4B)
3.c Ternary CH refined with riding coordinates:
 N1(H1)
3.d Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              49611
_shelx_hkl_checksum              45110
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'