A Tetrahydrofuran Ring-Opening Product: <i>trans</i>-Tetrachloro{4-[2-(phenylamino)pyridinio]butoxido-<i>O</i>}(tetrahydrofuran-<i>O</i>)zirconium(IV)
Polamo, Mika; Mutikainen, Ilpo; Leskelä, Markku; Acta Crystallographica Section C 53 (1997) 1036–1037; doi:10.1107/S0108270197003818

data_2006413
_publ_section_title
;A Tetrahydrofuran Ring-Opening Product:
 <i>trans</i>-Tetrachloro{4-[2-(phenylamino)pyridinio]butoxido-<i>O</i>}(tetrahydrofuran-<i>O</i>)zirconium(IV)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1036
_journal_page_last               1037
_journal_paper_doi               10.1107/S0108270197003818
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Zr Cl4 (C15 H18 N2 O) (C4 H8 O)]'
_chemical_formula_structural     '[Zr Cl4 (C4 H8 O) (C15 H18 N1 O1)'
_chemical_formula_sum            'C19 H26 Cl4 N2 O2 Zr'
_chemical_formula_weight         547.44
_chemical_name_systematic
;
trans-Tetrachloro-[4-(2-(phenylamino)pyridinium)butoxo-O]
(tetrahydrofuran-O)zirconium(IV)
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.251(5)
_cell_length_b                   11.548(5)
_cell_length_c                   14.280(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193.0(10)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2315.1(17)
_computing_cell_refinement       'Rigaku AFC7S software'
_computing_data_collection
'Rigaku AFC7S software (Molecular Structure Corporation, 1992a)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1992b)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      193.0(10)
_diffrn_measurement_device       'Rigaku AFC-7S diffractometer'
_diffrn_measurement_method       \w-2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3560
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   'psi-scan (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_hydrogen_treatment
'H atoms riding with U(H) = 1.3 U~eq~ of parent atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_obs          .0435
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0475P)^2^+1.7287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1057
_refine_ls_wR_factor_obs         .0994
_reflns_number_observed          2766
_reflns_number_total             3560
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1299.cif
_cod_data_source_block           zrapthf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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^)+(0.0475P)^2^+1.7287P] 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^)+(0.0475P)^2^+1.7287P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        '[ZrCl4 (C4 H8 O) (C15 H18 N2 O)]'
_cod_database_code               2006413