Direct synthesis of a {CoFe} dodecanuclear complex, revealing an unprecedented molecular structure type.
Chygorin, Eduard N.; Kokozay, Vladimir N.; Omelchenko, Irina V.; Shishkin, Oleg V.; Titiš, Ján; Boča, Roman; Nesterov, Dmytro S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10918–10922; doi:10.1039/c5dt01149c

data_7035217
_publ_section_title
;
 Direct synthesis of a {CoFe} dodecanuclear complex, revealing an
 unprecedented molecular structure type.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10918
_journal_page_last               10922
_journal_paper_doi               10.1039/c5dt01149c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C132 H146 Cl2 Co6 Fe6 N12 O36, 8(C3 H7 N O)'
_chemical_formula_sum            'C156 H202 Cl2 Co6 Fe6 N20 O44'
_chemical_formula_weight         3820.96
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-04-01 deposited with the CCDC.
2015-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.784(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.1418(13)
_cell_length_b                   13.1796(10)
_cell_length_c                   39.621(2)
_cell_measurement_reflns_used    5785
_cell_measurement_temperature    101.5
_cell_measurement_theta_max      28.1394
_cell_measurement_theta_min      2.8111
_cell_volume                     10505.4(12)
_computing_cell_refinement       'CrysAlis RED, Agilent Technologies, 2011'
_computing_data_collection       'CrysAlis CCD, Agilent Technologies, 2011'
_computing_data_reduction        'CrysAlis RED, Agilent Technologies, 2011'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      101.5
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   15.00   41.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -        0.5469   77.0000 -180.0000 26

  2 omega  -35.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.7774   77.0000  120.0000 88

  3 omega   -4.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8712   77.0000 -150.0000 61

  4 omega   61.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8712   77.0000 -150.0000 26

  5 omega   37.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8712   77.0000 -120.0000 77

  6 omega   -6.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8712   77.0000  -60.0000 73
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0110098000
_diffrn_orient_matrix_UB_12      0.0416024000
_diffrn_orient_matrix_UB_13      -0.0096766000
_diffrn_orient_matrix_UB_21      -0.0141014000
_diffrn_orient_matrix_UB_22      -0.0228265000
_diffrn_orient_matrix_UB_23      -0.0148905000
_diffrn_orient_matrix_UB_31      -0.0303291000
_diffrn_orient_matrix_UB_32      0.0255167000
_diffrn_orient_matrix_UB_33      0.0024332000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18347
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Agilent Technologies, 2011 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3964
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         18347
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                10814
_reflns_number_total             18347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01149c2.cif
_cod_data_source_block           koko451
_cod_depositor_comments          'Adding full bibliography for 7035217.cif.'
_cod_database_code               7035217
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O14-H14
 0.85 with sigma of 0.01
 O4S-H14
 1.75 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7S) \\sim Ueq, Uanis(C9S) \\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(C3S)
\\sim Ueq, Uanis(O1S) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(N1S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Riding coordinates:
 O14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
 H32B), C33(H33A,H33B), C43(H43A,H43B), C44(H44A,H44B), C54(H54A,H54B),
 C55(H55A,H55B), C65(H65A,H65B), C66(H66A,H66B)
4.c Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C3(H3), C4S(H4S), C4(H4), C5(H5), C6(H6), C7S(H7S), C7(H7),
 C10S(H10S), C14(H14A), C15(H15), C16(H16), C17(H17), C18(H18), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C36(H36), C37(H37), C38(H38), C39(H39),
  C40(H40), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62)
4.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC), C8S(H8SA,H8SB,H8SC), C9S(H9SA,H9SB,H9SC), C9(H9A,H9B,H9C), C11S(H11C,
 H11D,H11E), C12S(H12A,H12B,H12C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C),
 C42(H42A,H42B,H42C), C53(H53A,H53B,H53C), C64(H64A,H64B,H64C)
;
_olex2_submission_original_sample_id koko451
_olex2_submission_special_instructions 'No special instructions were received'