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_7027119
_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            'C16 H40 Br0.54 Cl1.46 Cu2 N8 P4 S4'
_chemical_formula_weight         818.67
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.11(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.649(1)
_cell_length_b                   15.064(1)
_cell_length_c                   9.682(1)
_cell_measurement_reflns_used    511
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      5.41
_cell_volume                     1694.6(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_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'
_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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13814
_diffrn_reflns_theta_max         30.18
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'none measured'
_exptl_absorpt_coefficient_mu    2.465
_exptl_absorpt_correction_T_max  0.78675
_exptl_absorpt_correction_T_min  0.44221
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Square plate'
_exptl_crystal_F_000             835
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.308
_refine_ls_goodness_of_fit_obs   1.323
_refine_ls_hydrogen_treatment    ref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.346
_refine_ls_restrained_S_obs      1.323
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.211
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.1714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0856
_refine_ls_wR_factor_obs         0.0790
_reflns_number_observed          4085
_reflns_number_total             4600
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807142jsup1.cif
_cod_data_source_block           (5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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.

'_exptl_absorpt_correction_type' value 'Integration'
changed to 'integration' 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:

'_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^)+(0.0000P)^2^+3.1714P] 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^)+(0.0000P)^2^+3.1714P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1694.7(2)
_cod_database_code               7027119