The synthesis and co-ordination chemistry of new functionalised pyridylphosphines derived from Ph2PCH2OH †
Durran, Sean E.; Smith, Martin B.; Slawin, Alexandra M. Z.; Steed, Jonathan W.; Journal of the Chemical Society, Dalton Transactions  (2000) 2771–; doi:10.1039/b003759l

data_7009810
_publ_section_title
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 The synthesis and co-ordination chemistry of new functionalised
 pyridylphosphines derived from Ph2PCH2OH&#x200A;&#x2020;
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_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2771
_journal_paper_doi               10.1039/b003759l
_journal_year                    2000
_chemical_compound_source        -
_chemical_formula_analytical     'C28.50 H31.50 Cl3.50 N2 O P Ru'
_chemical_formula_moiety         'C28 H31 Cl N2 O P Ru.Cl.[C H Cl3]0.5'
_chemical_formula_structural     'C28.50 H31.50 Cl3.50 N2 O P Ru'
_chemical_formula_sum            'C28.5 H31.5 Cl3.5 N2 O P Ru'
_chemical_formula_weight         674.17
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.8250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0689(7)
_cell_length_b                   12.2999(8)
_cell_length_c                   23.989(2)
_cell_measurement_reflns_used    84
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     3184.5(4)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.1712
_diffrn_reflns_av_sigmaI/netI    0.2870
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18840
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.856166
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       plate
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.852
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.2119
_refine_ls_R_factor_obs          0.0710
_refine_ls_shift/esd_max         0.050
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2502
_refine_ls_wR_factor_obs         0.1391
_reflns_number_observed          2761
_reflns_number_total             7483
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003759l.txt
_cod_data_source_block           6c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0576P)^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^)+(0.0576P)^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        3184.6(4)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C28.50 H31.50 Cl3.50 N2 O P Ru'
_cod_database_code               7009810