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_4330127
_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
'C88 H72 Co4 N16 O8 P2, C12 H10 O2 P, 5.45(C H4 O), Cl O4, 2.32(O)'
_chemical_formula_sum            'C105.45 H103.8 Cl Co4 N16 O21.77 P3'
_chemical_formula_weight         2307.66
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-01-28
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2010.12.31 svn.r1581, GUI svn.r3426)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4167(3)
_cell_length_b                   15.5390(3)
_cell_length_c                   52.5389(12)
_cell_measurement_reflns_used    5104
_cell_measurement_temperature    180.1
_cell_measurement_theta_max      77.0035
_cell_measurement_theta_min      2.5661
_cell_volume                     10953.4(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.1
_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  -52.00   20.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.8966   38.0000 -180.0000 72

  2 omega -118.00   -7.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.8966  -77.0000   30.0000 111

  3 omega    8.00   34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       39.8966  -84.0000  -76.0000 26

  4 omega   33.00   66.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -40.0000  -85.0000 33

  5 omega   42.00   71.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -45.0000   30.0000 29

  6 omega   96.00  177.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399   45.0000  150.0000 81

  7 omega   32.00  116.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399 -112.0000   53.0000 84

  8 omega   34.00   77.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -45.0000 -180.0000 43

  9 omega  105.00  147.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  125.0000   30.0000 42

 10 omega  103.00  141.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  112.0000  -33.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0581602000
_diffrn_orient_matrix_UB_12      0.0842687000
_diffrn_orient_matrix_UB_13      -0.0051578000
_diffrn_orient_matrix_UB_21      -0.0129750000
_diffrn_orient_matrix_UB_22      0.0236019000
_diffrn_orient_matrix_UB_23      0.0287452000
_diffrn_orient_matrix_UB_31      0.0982459000
_diffrn_orient_matrix_UB_32      -0.0466043000
_diffrn_orient_matrix_UB_33      0.0058256000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            33860
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.931
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       prism
_exptl_crystal_F_000             4771
_exptl_crystal_size_max          0.3144
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.0614
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881,8206 friedel pairs'
_refine_ls_abs_structure_Flack   -0.007(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1402
_refine_ls_number_reflns         18612
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                16753
_reflns_number_total             18612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014943_si_002_1.cif
_cod_data_source_block           exp_4
_cod_original_formula_sum        'C105.45 H103.80 Cl Co4 N16 O21.77 P3'
_cod_database_code               4330127
_chemical_oxdiff_formula         'Co4 N16 Cl1 C100 H60 P3 O21'
_reflns_odcompleteness_completeness 97.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97