Synthesis of cobalt cluster-based supramolecular triple-stranded helicates.
Yoo, Hyojong; Lee, Jeonghee; Kang, Philjae; Choi, Moon-Gun; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14213–14216; doi:10.1039/c5dt01895a

data_7035806
_publ_section_title
;
 Synthesis of cobalt cluster-based supramolecular triple-stranded
 helicates.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14213
_journal_page_last               14216
_journal_paper_doi               10.1039/c5dt01895a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C75 H57 Co8 N9 O42'
_chemical_formula_sum            'C75 H57 Co8 N9 O42'
_chemical_formula_weight         2227.73
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-07 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.945(2)
_cell_length_b                   23.945(2)
_cell_length_c                   17.1792(16)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      3.08
_cell_volume                     8530.3(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            79594
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.484
_diffrn_reflns_theta_min         2.919
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  0.4288
_exptl_absorpt_correction_T_min  0.2893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0852 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.6747.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             3366
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 3351 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10527
_refine_ls_number_restraints     810
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0902P)^2^+11.0764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.855
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.992
_reflns_number_gt                8263
_reflns_number_total             10527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01895a2.cif
_cod_data_source_block           supramolecule
_cod_depositor_comments
'Adding full bibliography for 7035806--7035807.cif.'
_cod_original_cell_volume        8530.6(18)
_cod_database_code               7035806
_audit_block_doi                 10.5517/cc14n6tt
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.636
_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, All O(H,H) groups
2. Restrained planarity
 C30, C31, C32, C33, C34, C35
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of
0.03 and sigma for terminal atoms of 0.001
Uanis(C41) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O17(0.5) O17A(0.5) O18(0.5) O18A(0.5) O21(0.5) H21A(0.5) H21B(0.5)
 O22(0.5) N5(0.5) C30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5) C33(0.5)
 H33(0.5) C34(0.5) C35(0.5) H35(0.5) C36(0.5) C36A(0.5) C40(0.5) H40(0.5)
 C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
6.a Rotating group:
 O19(H19A,H19B), O21(H21A,H21B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C16(H16), C17(H17),
 C18(H18), C23(H23), C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33),
  C35(H35), C37(H37), C40(H40)
6.c Fitted hexagon refined as free rotating group:
 C30(C31,C32,C33,C34,C35)
6.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C)
;
_smtbx_masks_special_details
;
The voids contained disordered
DMF with the partial occupancy. A satisfactory disorder model for
the solvent was not found, and therefore the Olex2 Solvent Mask routine
was used to mask out disordered density. The masked electron density of
156.3 e- per unit cell could be interpreted as 4 DMF (160 e-).'
;
_shelx_res_checksum              18832
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'