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_7226074
_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_moiety         'C88 H66 Cr6 N8 Na2 O28 2(H3 O1) 4(C2 H3 N)'
_chemical_formula_sum            'C96 H88 Cr6 N12 Na2 O30'
_chemical_formula_weight         2237.68
_chemical_name_common            '[Na3Cr6]-(2)'
_chemical_name_systematic        'complex 2'
_chemical_properties_physical    ', Hygroscopic'
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-07-21 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.553(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.8061(18)
_cell_length_b                   12.4863(14)
_cell_length_c                   22.4726(18)
_cell_measurement_reflns_used    1898
_cell_measurement_temperature    193.0(9)
_cell_measurement_theta_max      20.5510
_cell_measurement_theta_min      3.2980
_cell_volume                     4994.5(9)
_computing_cell_refinement
;
'Thu Jun 20 11:54:14 2013'
;
_computing_data_collection
;
'Thu Jun 20 11:54:14 2013'
;
_computing_data_reduction
;
'Thu Jun 20 11:54:14 2013'
;
_computing_molecular_graphics    'ORTEX (P. McArdle, 1995)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      193.0(9)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1742
_diffrn_reflns_av_unetI/netI     0.2095
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31838
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.811
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
crysalispro, agilent technologies,
version 1.171.36.24 (release 03-12-2012 crysalis171 .net)
(compiled dec  3 2012,18:21:49)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             2288
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.131
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         9115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.2046
_refine_ls_R_factor_gt           0.0967
_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^)+(0.1201P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.3020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4123
_reflns_number_total             9115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14811e2.cif
_cod_data_source_block           eh346a1
_cod_database_code               7226074
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.761
_shelxl_version_number           2014-1
_shelx_res_checksum              85664