Synthesis and reactions of metallo-diethynylbenzenes: building blocks for redox-active poly(phenyleneethynylene)s†
John, Kevin D.; Hopkins, Michael D.; Chemical Communications  (1999) 589–; doi:10.1039/a809231a

data_7110422
_publ_section_title
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 Synthesis and reactions of metallo-diethynylbenzenes: building blocks for
 redox-active poly(phenyleneethynylene)s&#x2020;
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              589
_journal_paper_doi               10.1039/a809231a
_journal_year                    1999
_chemical_formula_sum            'C37 H100 Cl P4 Si W'
_chemical_formula_weight         916.44
_chemical_name_systematic
;
 ?
;
_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                 95.23(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.977(9)
_cell_length_b                   30.300(30)
_cell_length_c                   16.449(20)
_cell_measurement_temperature    213(2)
_cell_volume                     4456(8)
_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      213(2)
_diffrn_measurement_device       'Siemens P3'
_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  0.1435
_diffrn_reflns_av_sigmaI/netI    0.1877
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5218
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.83
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.847
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.076
_refine_diff_density_min         -2.202
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.2602
_refine_ls_R_factor_obs          0.1279
_refine_ls_shift/esd_max         0.237
_refine_ls_shift/esd_mean        0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1406P)^2^+246.5966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4043
_refine_ls_wR_factor_obs         0.2812
_reflns_number_observed          2117
_reflns_number_total             4784
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809231asup1.cif
_cod_data_source_block           compound7
_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.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1406P)^2^+246.5966P] 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^)+(0.1406P)^2^+246.5966P] 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        4455.4(82)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110422