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_7035591
_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_absolute_configuration ad
_chemical_formula_moiety         'C43 H40 N P2 Ru, F6 P'
_chemical_formula_sum            'C43 H40 F6 N P3 Ru'
_chemical_formula_weight         878.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-13
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2015-05-06 deposited with the CCDC.
2015-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   14.287(2)
_cell_length_b                   21.502(4)
_cell_length_c                   37.246(6)
_cell_measurement_reflns_used    7414
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.37
_cell_volume                     11442(3)
_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
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_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  0.0800
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            158766
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.09
_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    0.600
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.4552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0704 before and 0.0498 after correction.
The Ratio of minimum to maximum transmission is 0.5127.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.057(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1455
_refine_ls_number_reflns         30397
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+19.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                25573
_reflns_number_total             30397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01806d1.cif
_cod_data_source_block           2c_13srv025
_cod_depositor_comments
'Adding full bibliography for 7035590--7035593.cif.'
_cod_database_code               7035591
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H6B of C6B, H45 of C45, H15A of C15A, H45A of C45A, H23B of C23B, H43 of
  C43, H14A of C14A, H62 of C62, H54 of C54, H33 of C33, H22 of C22, H23 of C23,
   H64B of C64B, H46 of C46, H4B of C4B, H26A of C26A, H14B of C14B, H26 of C26,
   H33A of C33A, H44A of C44A, {H1BA,H1BB} of N1B, H7B of C7B, H15B of C15B,
  H53 of C53, H33B of C33B, H45B of C45B, H34B of C34B, H35 of C35, H63B of
  C63B, H12A of C12A, {H1A,H1B} of N1, H54B of C54B, H56B of C56B, H53B of C53B,
   H52B of C52B, H16A of C16A, H54A of C54A, H22A of C22A, {H1AA,H1AB} of N1A,
  H4A of C4A, H56A of C56A, H6A of C6A, H62A of C62A, H36B of C36B, H42B of
  C42B, H3A of C3A, H63A of C63A, H65A of C65A, H65 of C65, H42A of C42A, H7A
  of C7A, H46A of C46A, H52 of C52, H25B of C25B, H63 of C63, H35A of C35A,
  H65B of C65B, H16B of C16B, H55 of C55, H34A of C34A, H43B of C43B, H55A of
  C55A, H42 of C42, H53A of C53A, H24A of C24A, H32A of C32A, H5A of C5A, H12B
  of C12B, H56 of C56, H36A of C36A, H32B of C32B, H64A of C64A, H24B of C24B,
  H35B of C35B, H55B of C55B, H66B of C66B, H66 of C66, H26B of C26B, H25A of
  C25A, H3B of C3B, H25 of C25, H44 of C44, H5B of C5B, H32 of C32, H43A of
  C43A, H46B of C46B, H52A of C52A, H22B of C22B, H44B of C44B, H3 of C3, H4 of
  C4, H5 of C5, H6 of C6, H7 of C7, H23A of C23A, H66A of C66A, H36 of C36,
  H13A of C13A, H24 of C24, H13B of C13B, H12 of C12, H13 of C13, H14 of C14,
  H15 of C15, H16 of C16, H62B of C62B, H64 of C64, H34 of C34
 At 1.5 times of:
  {H2AA,H2AB,H2AC} of C2A, {H2A,H2B,H2C} of C2, {H2BA,H2BB,H2BC} of C2B
2. Restrained distances
 P5A-F3BB , P5B-F3BA , P5A-F5BB , P5B-F5BA , P5B-F2BB , P5A-F2BA , P5B-F6BA ,
 P5A-F6BB , P5B-F4BB , P5A-F1BB , P5B-F1BA , P5A-F4BA
 with sigma of 0.005
3. Others
 Fixed Sof: P5B(0.5) F1BB(0.5) F2BA(0.5) F2BB(0.5) F3BA(0.5) F3BB(0.5)
 F4BA(0.5) F4BB(0.5) F5BB(0.5) F6BA(0.5) F6BB(0.5) P5A(0.5) F5BA(0.5) F1BA(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), 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), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), C3A(H3A), C4A(H4A), C5A(H5A),
 C6A(H6A), C7A(H7A), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A),
  C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C32A(H32A),
 C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C42A(H42A), C43A(H43A),
 C44A(H44A), C45A(H45A), C46A(H46A), C52A(H52A), C53A(H53A), C54A(H54A),
 C55A(H55A), C56A(H56A), C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A),
 C66A(H66A), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C12B(H12B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C22B(H22B), C23B(H23B),
 C24B(H24B), C25B(H25B), C26B(H26B), C32B(H32B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C42B(H42B), C43B(H43B), C44B(H44B), C45B(H45B),
 C46B(H46B), C52B(H52B), C53B(H53B), C54B(H54B), C55B(H55B), C56B(H56B),
 C62B(H62B), C63B(H63B), C64B(H64B), C65B(H65B), C66B(H66B)
4.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N1A(H1AA,H1AB), N1B(H1BA,H1BB)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC)
;