Solvothermal Synthesis of Discrete Cages and Extended Networks Comprising {Cr(III)3O(O2CR)3(oxime)3}2- (R = H, CH3, C(CH3)3, C14H9) Building Blocks.
Jones, Leigh Fon; Comar, Priyanka; Pitak, Mateusz; Coles, Simon; G. Ryder, Alan; Piligkos, Stergios; Brechin, Euan K.; Houton, Edel; RSC Adv.  (2016) –; doi:10.1039/C6RA14811E

data_7226073
_publ_section_title
;
 Solvothermal Synthesis of Discrete Cages and Extended Networks Comprising
 {Cr(III)3O(O2CR)3(oxime)3}2- (R = H, CH3, C(CH3)3, C14H9) Building
 Blocks.
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA14811E
_journal_year                    2016
_chemical_formula_sum            'C36 H39 Cr3 N6 Na3 O19'
_chemical_formula_weight         1084.70
_chemical_name_common            '[Na2Cr3]n'
_chemical_name_systematic        'complex 5 '
_chemical_properties_physical    ', Hygroscopic'
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-20 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.5335(5)
_cell_length_b                   15.5335(5)
_cell_length_c                   36.608(2)
_cell_measurement_reflns_used    7176
_cell_measurement_temperature    150(3)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      4.0340
_cell_volume                     7649.7(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      150(3)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -22.00   13.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2966  -99.0000 -180.0000 35
  
  2 omega  -15.00   26.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2966  -99.0000  -90.0000 41
  
  3 omega  -76.00    5.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2966  -57.0000    0.0000 81
  
  4 omega   44.00   92.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7497  178.0000 -150.0000 48
  
  5 omega   -5.00   86.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7497   37.0000  -30.0000 91
  
  6 omega  -52.00   47.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7497  -37.0000  150.0000 99
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0140143000
_diffrn_orient_matrix_UB_12      0.0375207000
_diffrn_orient_matrix_UB_21      0.0049458000
_diffrn_orient_matrix_UB_22      -0.0311226000
_diffrn_orient_matrix_UB_23      0.0129864000
_diffrn_orient_matrix_UB_31      0.0505573000
_diffrn_orient_matrix_UB_32      0.0201230000
_diffrn_orient_matrix_UB_33      -0.0049980000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            21194
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             3324
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN '
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+53.3411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                2757
_reflns_number_total             3118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra14811e2.cif
_cod_data_source_block           an6b2sq
_cod_original_cell_volume        7649.8(6)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7226073