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_7226075
_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         'C132 H198 Cr6 N12 Na4 O26'
_chemical_formula_sum            'C132 H198 Cr6 N12 Na4 O26'
_chemical_formula_weight         2772.97
_chemical_name_common            '[Na4Cr6]-3'
_chemical_name_systematic        'complex 3 '
_chemical_properties_physical    ', Hygroscopic'
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-20 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   26.9779(12)
_cell_length_b                   26.9779(12)
_cell_length_c                   71.622(4)
_cell_measurement_reflns_used    3559
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.6060
_cell_measurement_theta_min      3.4400
_cell_volume                     45143(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_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  -83.00   25.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1403  -19.0000  120.0000 144
  
  2 omega  -78.00  -51.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1403 -178.0000  -90.0000 36
  
  3 omega   -8.00   24.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   77.0000 -120.0000 43
  
  4 omega   47.00   74.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   77.0000 -120.0000 36
  
  5 omega   46.00   92.50   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  178.0000   60.0000 62
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0205040000
_diffrn_orient_matrix_UB_12      -0.0089916000
_diffrn_orient_matrix_UB_21      0.0164244000
_diffrn_orient_matrix_UB_22      0.0189476000
_diffrn_orient_matrix_UB_23      -0.0072792000
_diffrn_orient_matrix_UB_31      0.0152227000
_diffrn_orient_matrix_UB_32      0.0219582000
_diffrn_orient_matrix_UB_33      0.0066512000
_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  0.2348
_diffrn_reflns_av_unetI/netI     0.1838
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            59449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.972
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70988
_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    1.224
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             17640
_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          0.04
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         8855
_refine_ls_number_restraints     1286
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1972
_refine_ls_R_factor_gt           0.0907
_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^)+(0.0967P)^2^+38.8728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4076
_reflns_number_total             8855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14811e2.cif
_cod_data_source_block           EH458A7_rev1
_cod_original_cell_volume        45143(5)
_cod_database_code               7226075
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C6
 1.54 with sigma of 0.01
 C5-C8
 1.54 with sigma of 0.01
 C5-C8A
 1.54 with sigma of 0.01
 C5-C6A
 1.54 with sigma of 0.01
 C5-C7A
 1.54 with sigma of 0.01
 C37-C40A
 1.54 with sigma of 0.01
 C37-C38
 1.54 with sigma of 0.01
 C37-C38A
 1.54 with sigma of 0.01
 C37-C39
 1.54 with sigma of 0.01
 C37-C39A
 1.54 with sigma of 0.01
 C37-C40
 1.54 with sigma of 0.01
 C5-C7
 1.54 with sigma of 0.01
 C39A-C38A
 2.5 with sigma of 0.02
 C38A-C40A
 2.5 with sigma of 0.02
 C39A-C40A
 2.5 with sigma of 0.02
 C39-C38
 2.5 with sigma of 0.02
 C38-C40
 2.5 with sigma of 0.02
 C40-C39
 2.5 with sigma of 0.02
 C8-C7
 2.5 with sigma of 0.02
 C7-C6
 2.5 with sigma of 0.02
 C6-C8
 2.5 with sigma of 0.02
 C6A-C8A
 2.5 with sigma of 0.02
 C8A-C7A
 2.5 with sigma of 0.02
 C7A-C6A
 2.5 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C6A) = Uanis(C6)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(2)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
7.a Me refined with riding coordinates:
 C38A(H38D,H38E,H38F)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C9(H9), C16(H16), C18(H18), C24(H24)
7.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C6A(H6AA,
 H6AB,H6AC), C40A(H40D,H40E,H40F), C39A(H39D,H39E,H39F)
;
_shelx_res_checksum              373
_shelx_fab_checksum              10316
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'