Synthesis and characterisation of unsymmetrical metal (RuII, OsII) and ferrocenyl complexes of 1,3,5-triethynylbenzene
Long, Nicholas J.; Martin, Angela J.; White, Andrew J. P.; Williams, David J.; Fontani, Marco; Laschi, Franco; Zanello, Piero; Journal of the Chemical Society, Dalton Transactions  (2000) 3387–; doi:10.1039/b005186l

data_7010031
_publ_section_title
;
 Synthesis and characterisation of unsymmetrical metal (RuII, OsII) and
 ferrocenyl complexes of 1,3,5-triethynylbenzene
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3387
_journal_paper_doi               10.1039/b005186l
_journal_year                    2000
_chemical_formula_sum            'C86.5 H71 Cl Fe2 O1.5 P4 Ru'
_chemical_formula_weight         1506.53
_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                 109.633(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.377(4)
_cell_length_b                   10.2787(10)
_cell_length_c                   22.969(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      4.11
_cell_volume                     7421.9(15)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_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      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_av_sigmaI/netI    0.1309
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10144
_diffrn_reflns_theta_max         60.04
_diffrn_reflns_theta_min         1.41
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.227
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4418
_exptl_absorpt_correction_type   'Lamina [1 0 0]'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       plates
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.117
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         8634
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.138
_refine_ls_restrained_S_obs      1.157
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_obs          0.0983
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1738P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3165
_refine_ls_wR_factor_obs         0.2455
_reflns_number_observed          5844
_reflns_number_total             9878
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b005186l.txt
_cod_data_source_block           NL9806
_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^)+(0.1738P)^2^+0.0000P] 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^)+(0.1738P)^2^+0.0000P] 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        7421.8(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C86.50 H71 Cl Fe2 O1.50 P4 Ru'
_cod_database_code               7010031