Solid-State Self-Assembly of Triazolylpyridine-Based Helicates and Mesocate: Control of the Metal‒Metal Distances
Stevenson, Kristina A.; Melan, Caroline F. C.; Fleischel, Olivier; Wang, Ruiyao; Petitjean, Anne; Crystal Growth & Design 12 (2012) 5169–; doi:10.1021/cg301197w

data_4506985
_publ_section_title
;
 Solid-State Self-Assembly of Triazolylpyridine-Based Helicates and
 Mesocate: Control of the Metal--Metal Distances
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5169
_journal_paper_doi               10.1021/cg301197w
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C67 H66 B4 F16 Fe2 N28 O4'
_chemical_formula_weight         1786.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.553(3)
_cell_length_b                   14.553(3)
_cell_length_c                   68.745(16)
_cell_measurement_reflns_used    1581
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20.16
_cell_measurement_theta_min      2.80
_cell_volume                     12609(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12493
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.9739
_exptl_absorpt_correction_T_min  0.9364
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Difference electron density maps revealed the presence 
of disordered BF4- anions along with disordered lattice 
solvate CH3CN and water molecules, which were ultimately 
modeled through the use of the SQUEEZE subroutine of the 
PLATON software suite. PLATON Reference: P. v.d. Sluis & A.L. Spek. 
Acta Cryst. (1990), A46, 194. One solvent/anion accessible 
void per lattice were found, comprising a total volume 
of 4815 A3 and contributing a total of 1759 electrons. The 
void was thus assigned to 24 disordered BF4- anions, 24 water, 
and 24 chloroform, which contribute a total of 1776 electrons, 
and occupy about 4320 &#x00C5;3 in space. The larger volume and 
the smaller of the number of the electrons of the void 
may be a result of the disorder. The contributions have 
been included in all derived crystal quantities.
;
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                1827
_reflns_number_total             2757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301197w_si_003.cif
_cod_data_source_block           ap26a
_cod_original_cell_volume        12608(5)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               4506985