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_7226076
_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         'C62 H63 Cr6 N7 Na3 O26 1(H3 O1)'
_chemical_formula_sum            'C62 H66 Cr6 N7 Na3 O27'
_chemical_formula_weight         1719.16
_chemical_name_common            '[Na3Cr6]-4'
_chemical_name_systematic        'complex 4 '
_chemical_properties_physical    ', Hygroscopic'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 113.736(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3193(11)
_cell_length_b                   13.1295(5)
_cell_length_c                   22.7708(12)
_cell_measurement_reflns_used    3096
_cell_measurement_temperature    149.8(3)
_cell_measurement_theta_max      28.5480
_cell_measurement_theta_min      3.3080
_cell_volume                     7203.0(6)
_computing_cell_refinement
;
'Wed Oct 16 09:47:02 2013'
;
_computing_data_collection
;
'Wed Oct 16 09:47:02 2013'
;
_computing_data_reduction
;
'Wed Oct 16 09:47:02 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      149.8(3)
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14105
_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         25.349
_diffrn_reflns_theta_min         2.973
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95320
_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.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             3508
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN '
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0648P)^2^+5.0930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4621
_reflns_number_total             6590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14811e2.cif
_cod_data_source_block           eh429e1
_cod_database_code               7226076
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2014-1
_shelx_res_checksum              83227