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_4506988
_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            'C93 H92.5 B4 F16 Fe2 N26.5 O2.5'
_chemical_formula_weight         2080.38
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.648(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   51.649(3)
_cell_length_b                   14.9251(8)
_cell_length_c                   26.5830(15)
_cell_measurement_reflns_used    7104
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      21.80
_cell_measurement_theta_min      2.40
_cell_volume                     19416.1(19)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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  0.1134
_diffrn_reflns_av_sigmaI/netI    0.1115
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            86864
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9433
_exptl_absorpt_correction_T_min  0.9254
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered 
lattice solvate molecules, CH3CN and Et2O, 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 big solvent accessible void per lattice were found, comprising a 
total volume of 5771 A3 and contributing a total of 1231 electrons. 
The void was thus assigned to 20 CH3CN and 20 Et2O, which 
contribute 20 x (22 + 42) = 1280 electrons, and ocuppy about 3200 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 
although the precise composition of the lattice solvate is somewhat 
speculative.
;
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         19070
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1493
_refine_ls_R_factor_gt           0.0890
_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^)+(0.1473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2585
_reflns_number_gt                9090
_reflns_number_total             19070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301197w_si_006.cif
_cod_data_source_block           ap35a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_original_formula_sum        'C93 H92.50 B4 F16 Fe2 N26.50 O2.50'
_cod_database_code               4506988