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_4348553
_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         'C7 H2 Bi2 O15, C2 H O4, H2 O, C3 H12 N2'
_chemical_formula_sum            'C12 H17 Bi2 N2 O20'
_chemical_formula_weight         927.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 114.520(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2321(4)
_cell_length_b                   11.4820(2)
_cell_length_c                   13.4913(4)
_cell_measurement_reflns_used    4264
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9030
_cell_measurement_theta_min      3.8340
_cell_volume                     2146.77(12)
_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      N~2~
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -53.00   42.00   1.0000    5.6300
omega____ theta____ kappa____ phi______ frames
    -       15.0575  -77.0000  -30.0000 95

  2 omega  -12.00   83.00   1.0000    5.6300
omega____ theta____ kappa____ phi______ frames
    -       15.0575   77.0000  -90.0000 95

  3 omega   -2.00   79.00   1.0000    5.6300
omega____ theta____ kappa____ phi______ frames
    -       15.0575   57.0000  -90.0000 81

  4 omega    6.00   45.00   1.0000    5.6300
omega____ theta____ kappa____ phi______ frames
    -      -15.9950   38.0000 -150.0000 39
;
_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      0.0012046000
_diffrn_orient_matrix_UB_12      -0.0023838000
_diffrn_orient_matrix_UB_13      0.0530853000
_diffrn_orient_matrix_UB_21      -0.0511741000
_diffrn_orient_matrix_UB_22      0.0002698000
_diffrn_orient_matrix_UB_23      -0.0226978000
_diffrn_orient_matrix_UB_31      -0.0002619000
_diffrn_orient_matrix_UB_32      -0.0617193000
_diffrn_orient_matrix_UB_33      -0.0021416000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13357
_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         26.371
_diffrn_reflns_theta_min         3.434
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33968
_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    2.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.999
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0229P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3866
_reflns_number_total             4384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01341_si_005.cif
_cod_data_source_block           1
_cod_original_cell_volume        2146.76(11)
_cod_database_code               4348553
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 OW2(HW2A,HW2B)
2.b Rotating group:
 OW1(HW1A,HW1B)
2.c Ternary CH refined with riding coordinates:
 C9(H9)
2.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.e Tetrahedral OH refined with riding coordinates:
 O17(H17)
2.f Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              27723
_shelx_hkl_checksum              45986
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'