Syntheses, crystal structures and non-linear optical properties of two novel windmill-shaped clusters: [M2Pd4S8(dppm)2]·4DMF (M = W or Mo)
Zheng, Hegen; Leung, Wa-Hung; Tan, Weilian; Long, Deliang; Ji, Wei; Chen, Jiutong; Xin, Feibo; Xin, Xinquan; Journal of the Chemical Society, Dalton Transactions  (2000) 2145–; doi:10.1039/b000616p

data_7009393
_publ_section_title
;
 Syntheses, crystal structures and non-linear optical properties of two
 novel windmill-shaped clusters: [M2Pd4S8(dppm)2]&#x00B7;4DMF
 (M&#x2005;=&#x2005;W or Mo)
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2145
_journal_paper_doi               10.1039/b000616p
_journal_year                    2000
_chemical_formula_sum            'C62 H72 N4 O4 P4 Pd4 S8 W2'
_chemical_formula_weight         2110.90
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.12
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0822(3)
_cell_length_b                   19.6074(3)
_cell_length_c                   14.4743(3)
_cell_measurement_reflns_used    7645
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.76
_cell_volume                     3684.14(13)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13223
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.425
_exptl_absorpt_correction_T_max  0.8249
_exptl_absorpt_correction_T_min  0.5069
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_obs          0.0441
_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^)+(0.0228P)^2^+15.7173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0922
_refine_ls_wR_factor_obs         0.0833
_reflns_number_observed          4847
_reflns_number_total             6204
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000616p.txt
_cod_data_source_block           '[W2Pd4S8(dppm)2]4DMF'
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+15.7173P] 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^)+(0.0228P)^2^+15.7173P] 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        3684.11(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009393