Enantioselective Synthesis of Tetranuclear Quadruple Helicates
Claire Deville; Alexandra Spyratou; Paulina Aguirre-Etcheverry; Céline Besnard; Alan F. Williams; Inorganic Chemistry 51 (2012) 8667–8669; doi:10.1021/ic3014943

data_4330130
_publ_contact_author_address
;Department of Inorganic and Analytical Chemistry
University of Geneva,
30, quai Ernest Ansermet
CH1211 Geneva 4 
Switzerland
;
_publ_contact_author_email       Alan.Williams@unige.ch
_publ_contact_author_fax         '++41 22 3796830'
_publ_contact_author_name        'Alan F. Williams'
_publ_contact_author_phone       '++41 22 3796425'
_publ_section_title
;
 Enantioselective Synthesis of Tetranuclear Quadruple Helicates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8667
_journal_page_last               8669
_journal_paper_doi               10.1021/ic3014943
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C68 H58 Co4 N16 O8, 2(C3 H8 O), 2.8(C2 H6 O1), 0.41(O), 2.04(C2 H3 O2)'
_chemical_formula_sum            'C83.68 H96.93 Co4 N16 O17.29'
_chemical_formula_weight         1839.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-27
_audit_creation_method
;
  Olex2 1.1-alpha
  (compiled 2011.08.21 svn.r1945, GUI svn.r3824)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5232(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.72917(11)
_cell_length_b                   25.2968(3)
_cell_length_c                   17.3108(2)
_cell_measurement_reflns_used    11718
_cell_measurement_temperature    179.9
_cell_measurement_theta_max      73.2647
_cell_measurement_theta_min      2.5584
_cell_volume                     4683.75(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      179.9
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -88.00   -6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4365  -38.0000   90.0000 82

  2 omega  -69.00  -29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4365   38.0000  150.0000 40

  3 omega  -16.00   18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4365  101.0000  -94.0000 34

  4 omega  -59.00   20.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4365   38.0000  -60.0000 79

  5 omega   43.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       37.4365 -101.0000  160.0000 26

  6 omega   45.00   71.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000  -60.0000 26

  7 omega   31.00   66.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000   90.0000 35

  8 omega   37.00   76.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000  -90.0000 39

  9 omega  124.00  162.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -120.0000 38

 10 omega   88.00  114.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -120.0000 26

 11 omega   85.00  174.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000 -150.0000 89

 12 omega   26.00  146.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -77.0000   90.0000 120

 13 omega   81.00  165.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  150.0000 84

 14 omega   14.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6865 -111.0000   79.0000 26

 15 omega   49.00   75.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000 -180.0000 26

 16 omega  108.00  134.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000  120.0000 26

 17 omega   49.00   75.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000  -30.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0844462000
_diffrn_orient_matrix_UB_12      0.0486626000
_diffrn_orient_matrix_UB_13      -0.0156190000
_diffrn_orient_matrix_UB_21      -0.1129477000
_diffrn_orient_matrix_UB_22      -0.0317226000
_diffrn_orient_matrix_UB_23      0.0244534000
_diffrn_orient_matrix_UB_31      0.0290862000
_diffrn_orient_matrix_UB_32      0.0182415000
_diffrn_orient_matrix_UB_33      0.0844887000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18822
_diffrn_reflns_theta_full        73.42
_diffrn_reflns_theta_max         73.42
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    6.030
_exptl_absorpt_correction_T_max  0.454
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
    model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)  followed by 
a multi-scan correction
(abspack)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       prism
_exptl_crystal_F_000             1915
_exptl_crystal_size_max          0.4129
_exptl_crystal_size_mid          0.2181
_exptl_crystal_size_min          0.1806
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         11930
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0544
_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^)+(0.1022P)^2^+0.4959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1470
_reflns_number_gt                11284
_reflns_number_total             11930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014943_si_002_4.cif
_cod_data_source_block           claireacetatecu
_cod_original_cell_volume        4683.76(9)
_cod_database_code               4330130
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97