N-Heterocyclic Silyl Pincer Ligands
Dixon, Lily S. H.; Hill, Anthony F.; Sinha, Arup; Ward, Jas S.; Organometallics 33 (2014) 653–; doi:10.1021/om400792j

data_4082490
_publ_section_title
;
 N-Heterocyclic Silyl Pincer Ligands
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              653
_journal_paper_doi               10.1021/om400792j
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C57 H48 Cl1 N2 O1 P3 Ru1 Si1'
_chemical_formula_sum            'C57 H48 Cl N2 O P3 Ru Si'
_chemical_formula_weight         1034.55
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                80.3054(12)
_cell_angle_beta                 75.3846(8)
_cell_angle_gamma                82.5635(11)
_cell_formula_units_Z            2
_cell_length_a                   11.6868(2)
_cell_length_b                   14.0096(2)
_cell_length_c                   15.4974(3)
_cell_measurement_reflns_used    39910
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     2410.11(7)
_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 (Farrugia, 1997)'
_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  0.015
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21148
_diffrn_reflns_theta_full        27.537
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.691
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.45
_refine_diff_density_min         -0.68
_refine_ls_extinction_coef       197(18)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         11076
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.0019935
_refine_ls_shift/su_mean         0.0000447
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 3.17P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1013
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1013
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                9665
_reflns_number_total             11076
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      5.09
_oxford_refine_ls_r_factor_ref   0.0454
_oxford_refine_ls_scale          0.4631(6)
_oxford_reflns_number_all        11076
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om400792j_si_002.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/automatic-downloads/current/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/automatic-downloads/current/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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C57 H48 Cl1 N2 O1 P3 Ru1 Si1'
_cod_database_code               4082490
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
REM CONT CL(10, U[ISO]) UNTIL CL(11) 
REM CONT N(1, U'S) UNTIL N(2) 
REM CONT O(10, U[ISO]) UNTIL O(11) 
REM CONT P(1, U'S) UNTIL C(8) 
REM CONT C(10, U[ISO]) UNTIL C(11) 
REM CONT C(31, U'S) UNTIL C(336) 
CONT CL(10, OCC) CL(11, OCC) C(10, OCC) 
CONT C(11, OCC) O(10, OCC) O(11, OCC) 
EQUIV CL(10, OCC) CL(11, OCC) C(10, OCC) 
CONT C(11, OCC) O(10, OCC) O(11, OCC) 
WEIGHT -1 CL(11, OCC) C(11, OCC) O(11, OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) 
RIDE C   ( 214,X'S) H   (2141,X'S) 
RIDE C   ( 215,X'S) H   (2151,X'S) 
RIDE C   ( 216,X'S) H   (2161,X'S) 
RIDE C   ( 222,X'S) H   (2221,X'S) 
RIDE C   ( 223,X'S) H   (2231,X'S) 
RIDE C   ( 224,X'S) H   (2241,X'S) 
RIDE C   ( 225,X'S) H   (2251,X'S) 
RIDE C   ( 226,X'S) H   (2261,X'S) 
RIDE C   ( 312,X'S) H   (3121,X'S) 
RIDE C   ( 313,X'S) H   (3131,X'S) 
RIDE C   ( 314,X'S) H   (3141,X'S) 
RIDE C   ( 315,X'S) H   (3151,X'S) 
RIDE C   ( 316,X'S) H   (3161,X'S) 
RIDE C   ( 322,X'S) H   (3221,X'S) 
RIDE C   ( 323,X'S) H   (3231,X'S) 
RIDE C   ( 324,X'S) H   (3241,X'S) 
RIDE C   ( 325,X'S) H   (3251,X'S) 
RIDE C   ( 326,X'S) H   (3261,X'S) 
RIDE C   ( 332,X'S) H   (3321,X'S) 
RIDE C   ( 333,X'S) H   (3331,X'S) 
RIDE C   ( 334,X'S) H   (3341,X'S) 
RIDE C   ( 335,X'S) H   (3351,X'S) 
RIDE C   ( 336,X'S) H   (3361,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
VIBR 0.0, 0.02 = CL(10) TO CL(11) 
VIBR 0.0, 0.02 = C(10) TO C(11) 
VIBR 0.0, 0.02 = O(10) TO O(11) 
REM DIST 0.0, 0.02 = MEAN RU(1) TO CL(10), RU(1) TO CL(11) 
REM DIST 0.0, 0.02 = MEAN RU(1) TO C(10), RU(1) TO C(11) 
REM DIST 0.0, 0.02 = MEAN C(10) TO O(10), C(11) TO O(11) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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