Catalytic Synthesis of an Unsymmetrical PNP-Pincer-Type Phosphaalkene Ligand
Taguchi, Hiro-omi; Chang, Yung-Hung; Takeuchi, Katsuhiko; Ozawa, Fumiyuki; Organometallics 34 (2015) 1589–; doi:10.1021/acs.organomet.5b00195

data_4087511
_publ_section_title
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 Catalytic Synthesis of an Unsymmetrical PNP-Pincer-Type Phosphaalkene
 Ligand
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_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1589
_journal_paper_doi               10.1021/acs.organomet.5b00195
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C63.5 H83 Cl N P3 Ru'
_chemical_formula_weight         1089.74
_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                82.466(4)
_cell_angle_beta                 75.797(4)
_cell_angle_gamma                72.530(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4778(11)
_cell_length_b                   16.0104(18)
_cell_length_c                   18.230(2)
_cell_measurement_reflns_used    9383
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.1226
_cell_measurement_theta_min      2.5953
_cell_volume                     2822.5(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22982
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9579
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         12454
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+2.8886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                10722
_reflns_number_total             12454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00195_si_002.cif
_cod_data_source_block           complex_9
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' 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 
;
_cod_original_cell_volume        2822.5(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C63.50 H83 Cl N P3 Ru'
_cod_database_code               4087511