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_7027116
_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            'C18 H24 N4 P2 S2'
_chemical_formula_weight         422.47
_chemical_melting_point_gt       523
_chemical_name_systematic
; 
 butane-2,3-bis[(dimethylthiophosphoryl)hydrazide] 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                69.43(1)
_cell_angle_beta                 87.11(1)
_cell_angle_gamma                69.74(1)
_cell_formula_units_Z            2
_cell_length_a                   9.588(1)
_cell_length_b                   11.402(1)
_cell_length_c                   11.620(1)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.9
_cell_volume                     1112.1(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens SMART CCD detector'
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4911
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.88
_diffrn_standards_interval_time  '12 hours'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   'semi-empirical (equivalents)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       fragment
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0099(22)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_obs          0.0324
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.046P)^2^+0.67P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_obs         0.0846
_reflns_number_observed          3319
_reflns_number_total             3567
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807142jsup1.cif
_cod_data_source_block           L1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>523 K' was changed to
'523' - it should be numeric and without a unit designator.

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^)+(0.046P)^2^+0.67P] 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^)+(0.046P)^2^+0.67P] 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               7027116