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_4083039
_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        local
_chemical_formula_moiety         'C41 H62 Cl2 N2 O1 P2 Ru1'
_chemical_formula_sum            'C41 H62 Cl2 N2 O P2 Ru'
_chemical_formula_weight         832.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.5012(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8338(2)
_cell_length_b                   15.24170(10)
_cell_length_c                   23.7802(2)
_cell_measurement_reflns_used    131544
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     9000.68(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 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10316
_diffrn_reflns_theta_full        27.523
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.673
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_platon_squeeze_details
;
;
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.0042555
_refine_ls_shift/su_mean         0.0000440
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 33.7 54.9 32.8 13.6 3.09 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0910
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0910
_reflns_limit_h_max              32
_reflns_limit_h_min              -32
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                8765
_reflns_number_total             10316
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.60
_oxford_diffrn_Wilson_scale      57.85
_oxford_refine_ls_r_factor_ref   0.0426
_oxford_refine_ls_scale          0.14526(4)
_oxford_reflns_number_all        10314
_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 'Monoclinic' changed to 'monoclinic'
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.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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      'C 1 2/c 1 '
_cod_original_formula_sum        'C41 H62 Cl2 N2 O1 P2 Ru1'
_cod_database_code               4083039
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE RU(1, X'S, U'S) UNTIL C(74) 
CONT C(610, X'S, U'S, OCC) UNTIL C(661) 
EQUIV C(610, OCC), C(611, OCC), C(620, OCC), C(621, OCC) 
CONT C(630, OCC), C(631, OCC) C(640, OCC), C(641, OCC) 
CONT C(650, OCC), C(651, OCC), C(660, OCC), C(661, OCC) 
WEIGHT -1 C(610, OCC) C(620, OCC), C(630, OCC), C(640, OCC) 
CONT C(650, OCC), C(660, OCC) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  610,X'S) H   ( 6101,X'S) 
RIDE C   (  611,X'S) H   ( 6111,X'S) 
RIDE C   (  620,X'S) H   ( 6201,X'S) H   ( 6202,X'S) 
RIDE C   (  621,X'S) H   ( 6211,X'S) H   ( 6212,X'S) 
RIDE C   (  630,X'S) H   ( 6301,X'S) H   ( 6302,X'S) 
RIDE C   (  631,X'S) H   ( 6311,X'S) H   ( 6312,X'S) 
RIDE C   (  640,X'S) H   ( 6401,X'S) H   ( 6402,X'S) 
RIDE C   (  641,X'S) H   ( 6411,X'S) H   ( 6412,X'S) 
RIDE C   (  650,X'S) H   ( 6501,X'S) H   ( 6502,X'S) 
RIDE C   (  651,X'S) H   ( 6511,X'S) H   ( 6512,X'S) 
RIDE C   (  660,X'S) H   ( 6601,X'S) H   ( 6602,X'S) 
RIDE C   (  661,X'S) H   ( 6611,X'S) H   ( 6612,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;