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_7226072
_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         'C156 H96 Cr6 N6 Na O26, 2(C8 H20 N)'
_chemical_formula_sum            'C172 H136 Cr6 N8 Na O26'
_chemical_formula_weight         3065.87
_chemical_name_systematic        'Complex 1'
_chemical_properties_physical    ', Hygroscopic'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-16
_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                 121.745(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.800(2)
_cell_length_b                   17.2760(6)
_cell_length_c                   30.452(2)
_cell_measurement_reflns_used    6623
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.9000
_cell_measurement_theta_min      3.1380
_cell_volume                     17805.9(18)
_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_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (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 0.879
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_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  0.2071
_diffrn_reflns_av_unetI/netI     0.3321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            72141
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         29.180
_diffrn_reflns_theta_min         2.923
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77770
_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    1.144
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             6348
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH '
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         21163
_refine_ls_number_restraints     2210
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.2936
_refine_ls_R_factor_gt           0.1343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3164
_refine_ls_wR_factor_ref         0.4039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6544
_reflns_number_total             21163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14811e2.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        17805.9(19)
_cod_database_code               7226072
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C35
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.01
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
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.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C81(H81A,H81B), C83(H83A,H83B), C85(H85A,H85B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C52(H52), C53(H53),
  C54(H54), C55(H55), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62),
 C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C74(H74), C75(H75), C76(H76),
  C77(H77)
6.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,
 H86C)
;
_shelx_res_checksum              74916
_shelx_fab_checksum              93591
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'