Facile synthesis of unsymmetrical 9-phospha- and 9-arsafluorenes.
Diaz, Armando A.; Young, Jackie D.; Khan, Masood A.; Wehmschulte, Rudolf J.; Inorganic chemistry 45 (2006) 5568–5575; doi:10.1021/ic051976l

data_4350140
_publ_section_title
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 Facile synthesis of unsymmetrical 9-phospha- and 9-arsafluorenes.
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_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5568
_journal_page_last               5575
_journal_paper_doi               10.1021/ic051976l
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C34 H38 Cl5 P Ru'
_chemical_formula_weight         755.93
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.197(2)
_cell_angle_beta                 76.300(2)
_cell_angle_gamma                76.714(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0207(16)
_cell_length_b                   12.3536(18)
_cell_length_c                   12.8898(18)
_cell_measurement_reflns_used    6524
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.2
_cell_volume                     1642.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17310
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.7369
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.0332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                6154
_reflns_number_total             6745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051976lsi20051115_031734.cif
_cod_data_source_block           rw314m_COMPOUND_13.CHCl3
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350140