<i>N</i>,<i>N</i>-Diethylpyrrolidinium pentachloro(tetrahydrofuran)zirconate(IV)
Braunschweig, Holger; Kraft, Mario; Seeler, Fabian; Acta Crystallographica Section E 62 (2006) m3267–m3268; doi:10.1107/S1600536806045880

data_2211604
_publ_section_title
;
 <i>N</i>,<i>N</i>-Diethylpyrrolidinium
 pentachloro(tetrahydrofuran)zirconate(IV)
;
_journal_coeditor_code           SG2085
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3267
_journal_page_last               m3268
_journal_paper_doi               10.1107/S1600536806045880
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C8 H18 N) [Zr Cl5 (C4 H8 O)]'
_chemical_formula_moiety         'C8 H18 N +, C4 H8 Cl5 O Zr -'
_chemical_formula_sum            'C12 H26 Cl5 N O Zr'
_chemical_formula_weight         468.81
_chemical_name_systematic
;
N,N-Diethylpyrrolidinium pentachloro(tetrahydrofuran)zirconate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4148(17)
_cell_length_b                   14.9772(17)
_cell_length_c                   17.0633(19)
_cell_measurement_reflns_used    7412
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.1215
_cell_measurement_theta_min      2.6425
_cell_volume                     3939.4(8)
_computing_cell_refinement       'SAINT-NT (Bruker, 2003)'
_computing_data_collection       'SMART-NT (Bruker, 2003)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'XP in SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54795
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904.0
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.524
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3922
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+4.0936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                3440
_reflns_number_total             3922
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2085.cif
_cod_data_source_block           I
_cod_database_code               2211604
_cod_database_fobs_code          2211604