Synthesis and Solid-State Structures of Pyrazolylmethane Complexes of the Rare Earths
Andrea Sella; Sarah E. Brown; Jonathan W. Steed; Derek A. Tocher; Inorganic Chemistry 46 (2007) 1856–1864; doi:10.1021/ic062370f

data_4307863
_publ_section_title
;
Synthesis and Solid-State Structures of Pyrazolylmethane Complexes of the
Rare Earths
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1856
_journal_page_last               1864
_journal_paper_doi               10.1021/ic062370f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C31 H46 F9 Ho N6 O12 S3'
_chemical_formula_weight         1126.85
_chemical_name_common
'holmium(tris(3,5-dimethylpyrazolyl)methane) tris-(trifluoromethanesulfonate)'
_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                 95.481(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.2750(2)
_cell_length_b                   19.6570(10)
_cell_length_c                   19.8299(15)
_cell_measurement_temperature    120(2)
_cell_volume                     11359.1(10)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.748
_diffrn_measured_fraction_theta_max 0.748
_diffrn_measurement_device_type  KappaCCD
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.7974
_exptl_absorpt_correction_T_min  0.6484
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.891
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.00031(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+100.9406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.2027
_reflns_number_gt                5417
_reflns_number_total             7478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062370fsi20061212_110210_4.cif
_cod_data_source_block           ashol-2b
_cod_database_code               4307863