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_4330128
_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, Cl O4, C12 H10 O2 P, 5(C H4 O), 3.72(O)'
_chemical_formula_sum            'C105 H102 Cl Co4 N16 O22.72 P3'
_chemical_formula_weight         2315.58
_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             2012-02-06
_audit_creation_method
;
  Olex2 1.1-alpha
  (compiled 2011.08.21 svn.r1945, GUI svn.r3824)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4175(3)
_cell_length_b                   15.4982(6)
_cell_length_c                   52.7507(17)
_cell_measurement_reflns_used    7857
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      72.8650
_cell_measurement_theta_min      2.8483
_cell_volume                     10969.4(6)
_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, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.0
_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   16.00   51.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.8041   77.0000  150.0000 35

  2 omega -104.00  -78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.8041 -122.0000   61.0000 26

  3 omega  -76.00   12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.8041   77.0000  150.0000 88

  4 omega -109.00  -56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000  -45.0000 -120.0000 53

  5 omega   83.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.7256   45.0000  -60.0000 95

  6 omega  101.00  151.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.7256  111.0000 -150.0000 50

  7 omega   68.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.7256 -151.0000  170.0000 62

  8 omega  123.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.7256  111.0000  120.0000 52

  9 omega  107.00  156.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.7256  111.0000  150.0000 49
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0238444000
_diffrn_orient_matrix_UB_12      -0.0118632000
_diffrn_orient_matrix_UB_13      0.0283936000
_diffrn_orient_matrix_UB_21      -0.1116327000
_diffrn_orient_matrix_UB_22      -0.0076364000
_diffrn_orient_matrix_UB_23      -0.0063702000
_diffrn_orient_matrix_UB_31      0.0117018000
_diffrn_orient_matrix_UB_32      -0.0984014000
_diffrn_orient_matrix_UB_33      -0.0029071000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            27752
_diffrn_reflns_theta_full        72.83
_diffrn_reflns_theta_max         72.83
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.931
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.360
_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_colour_primary    pink
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             4783
_exptl_crystal_size_max          0.2597
_exptl_crystal_size_mid          0.1511
_exptl_crystal_size_min          0.1054
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1378
_refine_ls_number_reflns         18646
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1749
_reflns_number_gt                15232
_reflns_number_total             18646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014943_si_002_2.cif
_cod_data_source_block           wc05i
_cod_database_code               4330128
_chemical_oxdiff_formula         'C105 H103 Cl1 Co4 N16 O22 P3'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97