Dynamic NMR investigations of fluxionality of 2-(dimethoxymethyl)pyridine and 2,6-bis(dimethoxymethyl)pyridine in rhenium(I) and platinum(IV) complexes †
Creber, Michel L.; Orrell, Keith G.; Osborne, Anthony G.; Šik, Vladimir; Hursthouse, Michael B.; Abdul Malik, K. M.; Journal of the Chemical Society, Dalton Transactions  (2000) 4218–; doi:10.1039/b005821l

data_7010089
_publ_section_title
;
 Dynamic NMR investigations of fluxionality of
 2-(dimethoxymethyl)pyridine and 2,6-bis(dimethoxymethyl)pyridine in
 rhenium(I) and platinum(IV) complexes&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4218
_journal_paper_doi               10.1039/b005821l
_journal_year                    2000
_chemical_formula_sum            'C11 H20 I N O2 Pt'
_chemical_formula_weight         520.27
_chemical_name_systematic
;
 ?
;
_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_date             2000-07-19T14:42:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.66(2)
_cell_angle_beta                 73.25(2)
_cell_angle_gamma                87.47(3)
_cell_formula_units_Z            4
_cell_length_a                   8.939(2)
_cell_length_b                   12.575(5)
_cell_length_c                   14.183(4)
_cell_measurement_reflns_used    11814
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.24
_cell_volume                     1501.8(8)
_computing_cell_refinement
;
MADNESS
;
_computing_data_collection
;
MADNESS
;
_computing_data_reduction
;
ABSURD
;
_computing_molecular_graphics    'ORTEP-III (Burnett et al., 1996)'
_computing_publication_material  'WINGX (Farrugia (1998)'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.449
_diffrn_measured_fraction_theta_max 0.449
_diffrn_measurement_device
;
        Nonius FAST TV Area Detector
;
_diffrn_measurement_method       '\F and \w scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10864
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.387
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   none
_exptl_crystal_density_diffrn    2.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.573
_refine_diff_density_min         -2.475
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_gt    1.091
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3890
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      0.992
_refine_ls_restrained_S_gt       1.076
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          -0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1323
_refine_ls_wR_factor_gt          0.126
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                3030
_reflns_number_total             3890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005821l.txt
_cod_data_source_block           s92
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.0000P] 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^)+(0.0824P)^2^+0.0000P] 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-1
_cod_database_code               7010089