3,5-Dimethyl and 3,5-Di-tert-butylpyrazolato Complexes with Alkali Metals: Monomeric, Dimeric, Cluster, and 1D Chain Structures
Cortés-Llamas, Sara-Ángelica; Hernández-Lamoneda, Ramón; Velázquez-Carmona, Miguel-Ángel; Muñoz-Hernández, Miguel-Angel; Toscano, Rubén A.; Inorganic Chemistry 45 (2006) 286–294; doi:10.1021/ic051294y

data_4331635
_publ_section_title
;
 3,5-Dimethyl and 3,5-Di-tert-butylpyrazolato Complexes with Alkali
 Metals:&#x00A0; Monomeric, Dimeric, Cluster, and 1D Chain Structures
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              286
_journal_page_last               294
_journal_paper_doi               10.1021/ic051294y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C23 H43 N2 Na O6'
_chemical_formula_sum            'C23 H43 N2 Na O6'
_chemical_formula_weight         466.58
_chemical_name_systematic
; 
(3,5-di-tert-butylpyrazolato)(18-crown-6)sodium  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.414(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.903(2)
_cell_length_b                   19.174(4)
_cell_length_c                   14.314(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2578.8(9)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 6.23C (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL V 6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11357
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0377P)^2^+0.9277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                3648
_reflns_number_total             4619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051294ysup5.cif
_cod_data_source_block           Compound_4b
_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      'P 21/c'
_cod_database_code               4331635