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_7035807
_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
'0.33(C216 H156 Co25.54 N24 O129.08), 1.43(C3 H7 N O)'
_chemical_formula_sum            'C76.28 H62 Co8.51 N9.43 O44.45'
_chemical_formula_weight         2323.66
_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             2015-07-07
_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                   23.9077(5)
_cell_length_b                   23.9077(5)
_cell_length_c                   17.2642(5)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.45
_cell_measurement_theta_min      3.33
_cell_volume                     8545.8(4)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            147932
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.574
_diffrn_reflns_theta_min         3.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.158
_exptl_absorpt_correction_T_max  0.7405
_exptl_absorpt_correction_T_min  0.5580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1432 before and 0.1008 after correction.
The Ratio of minimum to maximum transmission is 0.7535.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic reddish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             3514
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 3646 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         11216
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1512P)^2^+2.2425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.860
_reflns_friedel_fraction_full    0.989
_reflns_friedel_fraction_max     0.989
_reflns_number_gt                9450
_reflns_number_total             11216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01895a2.cif
_cod_data_source_block           alpha-helix
_cod_depositor_comments
'Adding full bibliography for 7035806--7035807.cif.'
_cod_database_code               7035807
_audit_block_doi                 10.5517/cc14n6xx
_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 distances
 O20-H20B
 0.84 with sigma of 0.02
 O20-H20A
 0.84 with sigma of 0.02
 O20A-H20D
 0.84 with sigma of 0.02
 O20A-H20C
 0.84 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 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C40) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C39) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.001
5. Others
 Sof(Co5)=0.5*FVAR(2)
 Sof(O22)=FVAR(1)
 Sof(O23)=Sof(N5)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(O20A)=Sof(H20C)=Sof(H20D)=1-FVAR(3)
 Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(3)
6.a Riding coordinates:
 O20(H20A,H20B), O20A(H20C,H20D)
6.b Rotating group:
 O19(H19A,H19B)
6.c 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), C38(H38)
6.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_smtbx_masks_special_details
;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
436.9 e- per unit cell could be interpreted as 8 DMF (329 e-).'  
;
_shelx_res_checksum              38745
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'