Ruthenium and osmium complexes of dihydroperimidine-based N-heterocyclic carbene pincer ligands.
McQueen, Caitlin M. A.; Hill, Anthony F.; Ma, Chenxi; Ward, Jas S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20376–20385; doi:10.1039/c5dt03728j

data_7037570
_publ_section_title
;
 Ruthenium and osmium complexes of dihydroperimidine-based N-heterocyclic
 carbene pincer ligands.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20376
_journal_page_last               20385
_journal_paper_doi               10.1039/c5dt03728j
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C55 H56 Cl4 N2 P2 Ru2, C1 H1 Cl3'
_chemical_formula_sum            'C56 H57 Cl7 N2 P2 Ru2'
_chemical_formula_weight         1270.34
_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     other
_audit_creation_date             14-03-08
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2015-09-11 deposited with the CCDC.
2015-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                89.7761(16)
_cell_angle_beta                 89.3856(19)
_cell_angle_gamma                87.7982(12)
_cell_formula_units_Z            4
_cell_length_a                   14.8173(4)
_cell_length_b                   14.9752(4)
_cell_length_c                   24.0480(6)
_cell_measurement_reflns_used    234178
_cell_measurement_temperature    200
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.55
_cell_volume                     5331.8(2)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.077
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83082
_diffrn_reflns_theta_full        25.172
_diffrn_reflns_theta_max         25.172
_diffrn_reflns_theta_min         2.557
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/hexane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.71
_refine_diff_density_min         -2.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9609
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         18869
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.1155
_refine_ls_shift/su_max          0.0039584
_refine_ls_shift/su_mean         0.0002221
_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: 
 30.9 43.2 20.9 5.03 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2730
_refine_ls_wR_factor_gt          0.2513
_refine_ls_wR_factor_ref         0.2730
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                13227
_reflns_number_total             18877
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.49
_oxford_diffrn_Wilson_scale      70.23
_oxford_refine_ls_r_factor_ref   0.1534
_oxford_refine_ls_scale          0.14636(8)
_oxford_reflns_number_all        18869
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMA002 At 19:26 on 7/ 3'
_cod_data_source_file            c5dt03728j1.cif
_cod_data_source_block           CMA002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/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 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7037570
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
FIX CL(301,U[23]) 
FIX CL(301,U[33]) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM U(IJ) 0.0, 0.03 = CL(301) TO CL(302) 
REM U(IJ) 0.0, 0.03 = CL(302) TO CL(303) 
REM U(IJ) 0.0, 0.03 = CL(303) TO CL(301) 
REM 
U(IJ) 0.0, 0.01 = C(3) TO C(4) 
U(IJ) 0.0, 0.01 = C(3) TO C(5) 
REM 
U(IJ) 0.0, 0.03 = C(182) TO C(184) 
U(IJ) 0.0, 0.03 = C(184) TO C(186) 
U(IJ) 0.0, 0.03 = C(186) TO C(182) 
REM 
U(IJ) 0.0, 0.03 = C(51) TO C(52) 
U(IJ) 0.0, 0.03 = C(52) TO C(53) 
U(IJ) 0.0, 0.03 = C(53) TO C(54) 
U(IJ) 0.0, 0.03 = C(54) TO C(55) 
U(IJ) 0.0, 0.03 = C(55) TO C(56) 
U(IJ) 0.0, 0.03 = C(56) TO C(51) 
REM 
DIST 0.0, 0.005 = MEAN C(151) TO C(152), C(152) TO C(153) 
DIST 0.0, 0.005 = MEAN C(152) TO C(153), C(153) TO C(154) 
DIST 0.0, 0.005 = MEAN C(153) TO C(154), C(154) TO C(155) 
DIST 0.0, 0.005 = MEAN C(154) TO C(155), C(155) TO C(156) 
DIST 0.0, 0.005 = MEAN C(155) TO C(156), C(156) TO C(151) 
DIST 0.0, 0.005 = MEAN C(156) TO C(151), C(151) TO C(152) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;