Steric control of the formation of dinuclear double helicate and dinuclear meso-helicate assemblies
David J. Cooke; Jasmine M. Cross; Rebecca V. Fennessy; Lindsay P. Harding; Craig R. Rice; Christopher Slater; Chem.Commun. 49 (2013) 7785–; doi:10.1039/c3cc44611e

data_7109674
_publ_section_title
;
 Steric control of the formation of dinuclear double helicate and
 dinuclear meso-helicate assemblies
;
_journal_name_full               Chem.Commun.
_journal_page_first              7785
_journal_paper_doi               10.1039/c3cc44611e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C92 H64 N12 O2 S4 Zn2, 4(C F3 O3 S)(C H3 N O2) (C H3 C O2 C H2 C H3)'
_chemical_formula_sum            'C101 H75 F12 N13 O18 S8 Zn2'
_chemical_formula_weight         1926.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2013-07-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.746(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.525(4)
_cell_length_b                   24.073(2)
_cell_length_c                   12.188(1)
_cell_measurement_reflns_used    6298
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      22.38
_cell_measurement_theta_min      2.59
_cell_volume                     11443.9(18)
_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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.9829
_diffrn_measured_fraction_theta_max 0.9829
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53010
_diffrn_reflns_theta_full        28.4588
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1183
_exptl_crystal_F_000             3951.1988
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.7376
_refine_diff_density_min         -0.9178
_refine_diff_density_rms         0.1531
_refine_ls_d_res_high            0.7457
_refine_ls_d_res_low             11.4396
_refine_ls_goodness_of_fit_ref   0.9833
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    60
_refine_ls_number_parameters     578
_refine_ls_number_reflns         14217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9833
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.0033
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2419
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              52
_reflns_limit_h_min              -54
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                6799
_reflns_number_total             14217
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c3cc44611e.txt
_cod_data_source_block           mo_Chris_LOMeZn_DPA_0m
_cod_original_cell_volume        11443.7(18)
_cod_database_code               7109674
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C13(H13), C16(H16),
 C17(H17), C22(H22), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
  C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C34(H34a,H34b,H34c), C35(H35a,H35b,H35c)
;