Dihydroperimidine-Derived PNP Pincer Complexes as Intermediates en Route to N-Heterocyclic Carbene Pincer Complexes
Hill, Anthony F.; McQueen, Caitlin M. A.; Organometallics 33 (2014) 1909–; doi:10.1021/om5000985

data_4083040
_publ_section_title
;
 Dihydroperimidine-Derived PNP Pincer Complexes as Intermediates en Route
 to N-Heterocyclic Carbene Pincer Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1909
_journal_paper_doi               10.1021/om5000985
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C55 H47 Cl2 N2 P3 Ru, C H2 Cl2'
_chemical_formula_sum            'C56 H49 Cl4 N2 P3 Ru'
_chemical_formula_weight         1085.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                71.3895(12)
_cell_angle_beta                 76.4431(16)
_cell_angle_gamma                72.4232(16)
_cell_formula_units_Z            2
_cell_length_a                   11.3781(2)
_cell_length_b                   12.6054(4)
_cell_length_c                   18.8891(6)
_cell_measurement_reflns_used    36577
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     2418.91(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46625
_diffrn_reflns_theta_full        26.989
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9639
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11091
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0008686
_refine_ls_shift/su_mean         4.1432071
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 2.12P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0964
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0964
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7968
_reflns_number_total             11119
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.64
_oxford_diffrn_Wilson_scale      17.50
_oxford_refine_ls_r_factor_ref   0.0717
_oxford_refine_ls_scale          0.24142(11)
_oxford_reflns_number_all        11091
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om5000985_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083039--4083042.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4083040