Synthesis, Structure, and Thiolysis Reactions of Pyridine Soluble Alkaline Earth and Yttrium Thiolates
Andrew P. Purdy; Alan D. Berry; Clifford F. George; Inorganic Chemistry 36 (1997) 3370–3375; doi:10.1021/ic970045+

data_4327703
_publ_section_title
;
 Synthesis, Structure, and Thiolysis Reactions of Pyridine Soluble
 Alkaline Earth and Yttrium Thiolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3370
_journal_page_last               3375
_journal_paper_doi               10.1021/ic970045+
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'Y(NH2)3 + 3HSCEt3 in pyridine, recr PhMe'
_chemical_formula_analytical     'C31.1 H55.7 N1.88 S3.05 Y'
_chemical_formula_moiety         '(Y 3+)2, (Et3CS -)6, (C5H5N)4'
_chemical_formula_structural     (Y(SCEt3)3(C5H5N)2)2
_chemical_formula_sum            'C62 H108 N4 S6 Y2'
_chemical_formula_weight         1279.70
_chemical_name_common            'yttrium-t-heptylthiolate dipyridine dimer'
_chemical_name_systematic
;
 di-yttrium, tetrakis(3-ethyl-3-pentanethiolato-)-bis-(mu-3-ethyl-3-
 pentanethiolato-)tetrapyridine complex
;
_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
_cell_angle_alpha                81.612(7)
_cell_angle_beta                 79.546(5)
_cell_angle_gamma                78.169(7)
_cell_formula_units_Z            2
_cell_length_a                   11.5918(10)
_cell_length_b                   17.328(2)
_cell_length_c                   18.376(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      11.72
_cell_volume                     3530.0(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.1972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10050
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        -7.80
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.3603
_exptl_absorpt_correction_T_min  0.3189
_exptl_absorpt_correction_type   'semi empirical \Y scans xprep, siemens 94'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.1930
_refine_ls_R_factor_obs          0.0758
_refine_ls_shift/esd_max         0.032
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+3.3509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1631
_refine_ls_wR_factor_obs         0.1196
_reflns_number_observed          4312
_reflns_number_total             9192
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9700452B_2.cif
_cod_data_source_block
yttrium(iii)t-heptylthiolate_bis(pyridine)_complex
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'N/A' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+3.3509P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+3.3509P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3529.8(6)
_cod_database_code               4327703