Meso-Helicates with Rigid Angular Tetradentate Ligand: Design, Molecular Structures, and Progress Towards Self-Assembly of Metal-Organic Nanotubes
Rodrigue Djeda; Christophe Desmarets; Lise-Marie Chamoreau; Yanling Li; Yves Journaux; Geoffrey Gontard; Hani Amouri; Inorganic Chemistry 52 (2013) 13042–13047; doi:10.1021/ic4017195

data_4336714
_publ_contact_author
;
  Hani Amouri
;
_publ_contact_author_email       hani.amouri@upmc.fr
_publ_contact_author_fax         '00 33 1 44 27 38 41'
_publ_contact_author_phone       '00 33 1 44 27 30 83'
_publ_section_title
;
 Meso-Helicates with Rigid Angular Tetradentate Ligand: Design, Molecular
 Structures, and Progress Towards Self-Assembly of Metal-Organic Nanotubes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13042
_journal_page_last               13047
_journal_paper_doi               10.1021/ic4017195
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C94 H72 N16 Ni2, 4(B F4), 5(C2 H3 N)'
_chemical_formula_sum            'C104 H87 B4 F16 N21 Ni2'
_chemical_formula_weight         2095.60
_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_method           SHELXL-2013
_cell_angle_alpha                79.794(2)
_cell_angle_beta                 82.135(2)
_cell_angle_gamma                61.1010(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2211(5)
_cell_length_b                   12.3191(5)
_cell_length_c                   20.3835(8)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.21
_cell_volume                     2639.46(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Crystal Impact GbR, Bonn, Germany'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32696
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.074
_diffrn_reflns_theta_min         1.960
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. or Sheldrick, G. M. (1996)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10395
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+2.1488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7727
_reflns_number_total             10395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4017195_si_001_1.cif
_cod_data_source_block           rd071112_0m
_cod_database_code               4336714