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_4506986
_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            'C61 H68.5 B4 F16 Fe2 N28.5 O1.5'
_chemical_formula_weight         1683.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                109.529(3)
_cell_angle_beta                 101.269(3)
_cell_angle_gamma                103.509(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8629(5)
_cell_length_b                   17.9032(6)
_cell_length_c                   17.9445(10)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.30
_cell_volume                     3895.3(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56107
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_correction_T_min  0.8912
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered 
lattice solvate molecules and disordered BF4- anion, 
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. 
Two accessible voids per lattice were found, comprising a 
total volume of 582 A3 and contributing a total of 159 electrons. 
The voids were assigned to disordered 2BF4- and 3MeCN, which 
contribute 2 x 42 + 3 x 22 = 150 electrons, and ocuppy about 380 A3 in space. 
The larger volume of the void may be a result of the disorder. The
contributions have been included in all derived crystal quantities.
;
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         15271
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1077P)^2^+3.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                12314
_reflns_number_total             15271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301197w_si_004.cif
_cod_data_source_block           ap28a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C61 H68.50 B4 F16 Fe2 N28.50 O1.50'
_cod_database_code               4506986