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_4348555
_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         'C5 In O10, C6 H16 N2'
_chemical_formula_sum            'C11 H16 In N2 O10'
_chemical_formula_weight         451.08
_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                   25.1335(2)
_cell_length_b                   25.1335(2)
_cell_length_c                   9.74539(12)
_cell_measurement_reflns_used    5204
_cell_measurement_temperature    292.70(18)
_cell_measurement_theta_max      72.4190
_cell_measurement_theta_min      3.9530
_cell_volume                     6156.09(10)
_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      292.70(18)
_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    7.00  108.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   19.0000 -120.0000 101

  2 omega    1.00   75.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -30.0000 74

  3 omega   23.00   90.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -180.0000 67

  4 omega   18.00  106.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000 -150.0000 88

  5 omega   38.00   91.00   1.0000   10.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

  6 omega   38.00   91.00   1.0000   10.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

  7 omega   39.00  109.00   1.0000   10.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

  8 omega   81.00  176.00   1.0000   10.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

  9 omega   20.00   83.00   1.0000    2.7100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -30.0000 63
;
_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      0.0120302000
_diffrn_orient_matrix_UB_12      0.0509727000
_diffrn_orient_matrix_UB_13      0.0821311000
_diffrn_orient_matrix_UB_21      0.0333777000
_diffrn_orient_matrix_UB_22      -0.0326777000
_diffrn_orient_matrix_UB_23      0.1023512000
_diffrn_orient_matrix_UB_31      0.0500041000
_diffrn_orient_matrix_UB_32      0.0095051000
_diffrn_orient_matrix_UB_33      -0.0880829000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8423
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.018
_diffrn_reflns_theta_max         67.018
_diffrn_reflns_theta_min         4.867
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39831
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2540
_reflns_number_total             2742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01341_si_007.cif
_cod_data_source_block           1
_cod_original_cell_volume        6156.10(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4348555
_reflns_odcompleteness_completeness 99.93
_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, 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:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), N2(H2A,
 H2B)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              22589
_shelx_hkl_checksum              55897
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'