Solvent-free synthesis of new metal phosphate-oxalates: influence of different metal ions on the framework structures.
Luan, Lindong; Yang, Meng; Bian, Yixuan; Lin, Zhien; Huang, Hui; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13485–13489; doi:10.1039/c5dt01613d

data_7035617
_publ_section_title
;
 Solvent-free synthesis of new metal phosphate-oxalates: influence of
 different metal ions on the framework structures.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13485
_journal_page_last               13489
_journal_paper_doi               10.1039/c5dt01613d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C H3 Cd O7 P, C2 H7 N'
_chemical_formula_sum            'C3 H10 Cd N O7 P'
_chemical_formula_weight         315.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-03
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1156(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.63389(10)
_cell_length_b                   15.9428(2)
_cell_length_c                   9.61828(15)
_cell_measurement_reflns_used    4791
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.4750
_cell_measurement_theta_min      5.3640
_cell_volume                     863.75(2)
_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, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9797
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000   90.0000 67

  2 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -180.0000 84

  3 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000  150.0000 94

  4 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -60.0000 84

  5 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -90.0000 74

  6 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000 -150.0000 88

  7 omega   39.00  109.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 70

  8 omega   40.00   98.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

  9 omega   38.00   91.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

 10 omega   91.00  176.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 85

 11 omega   38.00  116.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 78

 12 omega   81.00  176.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

 13 omega  100.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 78

 14 omega  100.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 78

 15 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -120.0000 84

 16 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   30.0000 94

 17 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000  -30.0000 88

 18 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000    0.0000 84

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

 20 omega   91.00  176.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

 21 omega   87.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91
;
_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      -0.0135186000
_diffrn_orient_matrix_UB_12      -0.0863845000
_diffrn_orient_matrix_UB_13      -0.0714689000
_diffrn_orient_matrix_UB_21      -0.0816157000
_diffrn_orient_matrix_UB_22      -0.0398187000
_diffrn_orient_matrix_UB_23      0.1369433000
_diffrn_orient_matrix_UB_31      -0.2607205000
_diffrn_orient_matrix_UB_32      0.0169459000
_diffrn_orient_matrix_UB_33      -0.0424697000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.061
_diffrn_reflns_theta_max         67.061
_diffrn_reflns_theta_min         5.372
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31729
_exptl_absorpt_correction_type   numerical
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0764P)^2^+0.0960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1489
_reflns_number_total             1540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01613d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7035614--7035619.cif.'
_cod_database_code               7035617
_reflns_odcompleteness_completeness 99.88
_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,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 OW1(HW1A,HW1B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              88509
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'