Supramolecular assemblies prepared from an iron(II) tripodal complex, tetrafluoroborate, and alkali metal cations. The effect of cation size on coordination number, anion disorder and hydrogen bonding
Alvarado, Luigi; Brewer, Cynthia; Brewer, Greg; Butcher, Ray J.; Straka, Alison; Viragh, Carol; CrystEngComm 11 (2009) 2297–; doi:10.1039/b905061b

data_7201106
_publ_section_title
;
 Supramolecular assemblies prepared from an iron(II) tripodal complex,
 tetrafluoroborate, and alkali metal cations. The effect of cation size
 on coordination number, anion disorder and hydrogen bonding
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2297
_journal_paper_doi               10.1039/b905061b
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C18 H24 B3 Cs F12 Fe N10'
_chemical_formula_weight         829.66
_space_group_IT_number           147
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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            2
_cell_length_a                   13.4660(3)
_cell_length_b                   13.4660(3)
_cell_length_c                   9.4702(2)
_cell_measurement_reflns_used    10823
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.3833
_cell_measurement_theta_min      4.6155
_cell_volume                     1487.19(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21018
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.45
_diffrn_reflns_theta_min         4.62
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3421
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0450P)^2^+1.4010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                2518
_reflns_number_total             3421
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b905061b.txt
_cod_data_source_block           gab_a28x
_cod_database_code               7201106