Bifunctional dithiocarbamates: a bridge between coordination chemistry and nanoscale materials
Knight, Edward R.; Cowley, Andrew R.; Hogarth, Graeme; Wilton-Ely, James D. E. T.; Dalton Transactions  (2009) 607–; doi:10.1039/b814476a

data_7000345
_publ_section_title
;
 Bifunctional dithiocarbamates: a bridge between coordination chemistry
 and nanoscale materials
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              607
_journal_paper_doi               10.1039/b814476a
_journal_year                    2009
_chemical_formula_moiety
;
C92 H82 N2 P6 Pd Ru S4, C4 H10 O, 2(B F4), 3(C H2 Cl2)
;
_chemical_formula_sum            'C99 H98 B2 Cl6 F8 N2 O P6 Pd Ru S4'
_chemical_formula_weight         2239.78
_chemical_melting_point          ?
_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
_audit_creation_date             08-09-24
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                102.9433(6)
_cell_angle_beta                 92.8485(6)
_cell_angle_gamma                106.8897(6)
_cell_formula_units_Z            2
_cell_length_a                   13.9532(2)
_cell_length_b                   15.4074(2)
_cell_length_c                   25.2067(4)
_cell_measurement_reflns_used    75176
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     5015.09(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            75176
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         5.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.60
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0596
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         15431
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.000625
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.58 0.371 1.07
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0804
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0628
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                16889
_reflns_number_total             22434
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0590
_oxford_refine_ls_scale          0.3014(4)
_oxford_reflns_number_all        22434
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title arc1612
_cod_data_source_file            b814476a.txt
_cod_data_source_block           2
_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:

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

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C99 H98 B2 Cl6 F8 N2 O1 P6 Pd1 Ru1 S4'
_cod_database_code               7000345