Syntheses, structural characterisation and electronic structures of some simple acyclic amino carbene complexes.
Eaves, Samantha G.; Yufit, Dmitry S.; Skelton, Brian W.; Howard, Judith A. K.; Low, Paul J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14341–14348; doi:10.1039/c5dt01806d

data_7035592
_publ_section_title
;
 Syntheses, structural characterisation and electronic structures of some
 simple acyclic amino carbene complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14341
_journal_page_last               14348
_journal_paper_doi               10.1039/c5dt01806d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H44 N P2 Ru, 2(C H Cl3), F6 P'
_chemical_formula_sum            'C40 H46 Cl6 F6 N P3 Ru'
_chemical_formula_weight         1061.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-10
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Mar 21 2013 11:16:32, GUI svn.r4446)
;
_audit_update_record
;
2015-05-06 deposited with the CCDC.
2015-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                83.8710(10)
_cell_angle_beta                 76.3000(10)
_cell_angle_gamma                81.0140(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9534(6)
_cell_length_b                   13.4096(8)
_cell_length_c                   15.8099(9)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.99
_cell_measurement_theta_min      2.30
_cell_volume                     2222.5(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43327
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.33
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0534 before and 0.0226 after correction.
The Ratio of minimum to maximum transmission is 0.5923.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.371
_refine_diff_density_min         -1.956
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         11826
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                10787
_reflns_number_total             11826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01806d1.cif
_cod_data_source_block           2d_13s120
_cod_depositor_comments
'Adding full bibliography for 7035590--7035593.cif.'
_cod_database_code               7035592
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl5A-C2SA \\sim Cl5B-C2SB \\sim Cl4B-C2SB \\sim Cl4A-C2SA \\sim Cl6A-C2SA 
\\sim Cl6B-C2SB
 with sigma of 0.01
 C2A-C1 \\sim C2B-C1
 with sigma of 0.005
 P3-F1A \\sim P3-F1B \\sim P3-F4B \\sim P3-F4A \\sim P3-F6B \\sim P3-F6A 
\\sim P3-F2A \\sim P3-F2B
 with sigma of 0.01
3. Others
 Fixed Sof: C2A(0.4) H2AA(0.4) H2AB(0.4) H2AC(0.4) C2B(0.6) H2BA(0.6)
 H2BB(0.6) H2BC(0.6) Cl4A(0.5) Cl4B(0.5) Cl5A(0.5) Cl5B(0.5) Cl6A(0.5)
 Cl6B(0.5) C2SA(0.5) H2SA(0.5) C2SB(0.5) H2SB(0.5) F1A(0.6) F1B(0.4) 
F2A(0.6) F2B(0.4) F4A(0.4) F4B(0.6) F6A(0.4) F6B(0.6)
4.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2SA(H2SA), C2SB(H2SB)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), 
C46(H46),  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
4.d Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C10(H10A,H10B,H10C), C11(H11A,
H11B, H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;