Dimethylthiophosphoryl hydrazone ligands and their copper complexes: crystal structures and analysis of their solution complexation behaviour by electrospray mass spectrometry
Batsanov, Andrei S.; Churakov, Andrei V.; Easson, Morag A. M.; Govenlock, Linda J.; Howard, Judith A. K.; Moloney, Janet M.; Parker, David; Journal of the Chemical Society, Dalton Transactions  (1999) 323–; doi:10.1039/a807142j

data_7027118
_publ_section_title
;
 Dimethylthiophosphoryl hydrazone ligands and their copper complexes:
 crystal structures and analysis of their solution complexation behaviour
 by electrospray mass spectrometry
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              323
_journal_paper_doi               10.1039/a807142j
_journal_year                    1999
_chemical_formula_sum            'C8 H13 N2 P S'
_chemical_formula_weight         200.23
_chemical_melting_point          412.0(10)
_chemical_name_systematic
; 
 2-(dimethylthiophosphorylamino)-6-picoline 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 114.54(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.415(1)
_cell_length_b                   8.348(1)
_cell_length_c                   11.983(1)
_cell_measurement_reflns_used    447
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     1038.7(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'SHELXTL Vesion 5/VMS (1995)'
_computing_publication_material  'SHELXTL Vesion 5/VMS (1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_method       '\w scan in 0.3\% frames, 15 s/frame'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8012
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  '10 h'
_diffrn_standards_number         '178 (50 frames)'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.9518
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            'colourless        '
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       'lump              '
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.163
_refine_ls_goodness_of_fit_obs   1.151
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_restrained_S_obs      1.151
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_obs          0.0329
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.6285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0824
_refine_ls_wR_factor_obs         0.0727
_reflns_number_observed          2425
_reflns_number_total             2815
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807142jsup1.cif
_cod_data_source_block           L3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '411-413 K' was changed to
'412.0(10)' - the average value was taken and precision was
estimated.

'_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.6285P] 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^)+(0.0216P)^2^+0.6285P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7027118