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_4330129
_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_formula_moiety
'C88 H72 Co4 N16 O8 P2, 2(C12 H10 O2 P), 7.34699(C H4 O), 0.5(O)'
_chemical_formula_sum            'C119.35 H121.4 Co4 N16 O19.85 P4'
_chemical_formula_weight         2457.16
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-07-08
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                97.666(2)
_cell_angle_beta                 91.277(2)
_cell_angle_gamma                108.580(3)
_cell_formula_units_Z            2
_cell_length_a                   16.5412(5)
_cell_length_b                   19.2351(5)
_cell_length_c                   19.8514(5)
_cell_measurement_reflns_used    18874
_cell_measurement_temperature    159.6
_cell_measurement_theta_max      73.3403
_cell_measurement_theta_min      2.8227
_cell_volume                     5919.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      159.6
_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  -57.00   42.60   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4599   77.0000   60.0000 166

  2 omega  -73.00   44.00   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4599   77.0000  -60.0000 195

  3 omega  -73.00   44.00   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4599   77.0000 -180.0000 195

  4 omega  -55.00  -12.40   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.4599  -77.0000  -30.0000 71

  5 omega   14.00   41.00   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       37.4599   77.0000 -150.0000 45

  6 omega   51.00   87.60   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       37.4599   77.0000   90.0000 61

  7 omega    2.00   41.00   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       37.4599   77.0000   90.0000 65

  8 omega   60.00   85.80   0.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       37.4599   77.0000 -150.0000 43

  9 omega   80.00  128.60   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265   45.0000 -180.0000 81

 10 omega  108.00  153.60   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  111.0000   60.0000 76

 11 omega   32.00   63.80   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  -45.0000  -60.0000 53

 12 omega   45.00  118.80   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  -77.0000  -60.0000 123

 13 omega  105.00  156.60   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  111.0000  -30.0000 86

 14 omega  101.00  126.80   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  111.0000  -60.0000 43

 15 omega   84.00  109.80   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265 -109.0000   37.0000 43

 16 omega   32.00   57.80   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  -45.0000   90.0000 43

 17 omega  113.00  176.00   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  111.0000    0.0000 105

 18 omega   41.00   77.00   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  -45.0000    0.0000 60

 19 omega  116.00  149.00   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  111.0000 -150.0000 55

 20 omega   79.00  178.00   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265   43.0000   37.0000 165

 21 omega   79.00  175.60   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265   43.0000  113.0000 161

 22 omega   66.00  135.00   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265  -77.0000   30.0000 115

 23 omega   38.00  110.60   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265 -112.0000  -63.0000 121

 24 omega   59.00  122.60   0.6000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7265 -129.0000 -130.0000 106
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0381829000
_diffrn_orient_matrix_UB_12      -0.0693873000
_diffrn_orient_matrix_UB_13      0.0344443000
_diffrn_orient_matrix_UB_21      -0.0722748000
_diffrn_orient_matrix_UB_22      0.0294466000
_diffrn_orient_matrix_UB_23      0.0246598000
_diffrn_orient_matrix_UB_31      -0.0549438000
_diffrn_orient_matrix_UB_32      -0.0402275000
_diffrn_orient_matrix_UB_33      -0.0660790000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41928
_diffrn_reflns_theta_full        73.49
_diffrn_reflns_theta_max         73.49
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.431
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       prism
_exptl_crystal_F_000             2553
_exptl_crystal_size_max          0.4617
_exptl_crystal_size_mid          0.1443
_exptl_crystal_size_min          0.0824
_refine_diff_density_max         1.829
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1604
_refine_ls_number_reflns         23183
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1429P)^2^+1.5688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                20374
_reflns_number_total             23183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014943_si_002_3.cif
_cod_data_source_block           clairecomixn
_cod_original_formula_sum        'C119.35 H121.40 Co4 N16 O19.85 P4'
_cod_database_code               4330129
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97