Multimetallic arrays: Symmetrical bi-, tri- and tetrametallic complexes based on the group 10 metals and the functionalisation of gold nanoparticles with nickel-phosphine surface units
Knight, Edward R.; Leung, Nina H.; Lin, Yvonne H.; Cowley, Andrew R.; Watkin, David J.; Thompson, Amber L.; Hogarth, Graeme; Wilton-Ely, James D. E. T.; Dalton Transactions  (2009) 3688–3697; doi:10.1039/b821947h

data_7001258
_publ_section_title
;
 Multimetallic arrays: Symmetrical bi-, tri- and tetrametallic
 complexes based on the group 10 metals and the functionalisation of
 gold nanoparticles with nickel-phosphine surface units
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3688
_journal_page_last               3697
_journal_paper_doi               10.1039/b821947h
_journal_year                    2009
_chemical_formula_moiety         'C76.60 H69.20 B2 Cl5.20 F8 Fe2 N2 P4 Pd2 S4'
_chemical_formula_sum            'C76.6 H69.2 B2 Cl5.2 F8 Fe2 N2 P4 Pd2 S4'
_chemical_formula_weight         1952.42
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-02-26
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 97.2552(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5409(2)
_cell_length_b                   18.8334(3)
_cell_length_c                   21.2790(4)
_cell_measurement_reflns_used    45252
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     4190.51(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.081
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45252
_diffrn_reflns_theta_full        27.486
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         5.131
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1962.400
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.09
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0797
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000885
_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:
0.445 0.263 0.218
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0959
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0558
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                5911
_reflns_number_total             9827
_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   0.0483
_oxford_refine_ls_scale          0.08517(16)
_oxford_reflns_number_all        9537
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title arc1609
_cod_data_source_file            b821947h.txt
_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 2.4.1 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 21/n 1 '
_cod_original_formula_sum        'C76.60 H69.20 B2 Cl5.20 F8 Fe2 N2 P4 Pd2 S4'
_cod_database_code               7001258