Synthesis and coordination chemistry of tridentate (PNN) amine enamido phosphine ligands with ruthenium.
Wambach, T. C.; Lenczyk, C.; Patrick, B. O.; Fryzuk, M. D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5583–5589; doi:10.1039/c6dt00214e

data_7038429
_publ_section_title
;
 Synthesis and coordination chemistry of tridentate (PNN) amine enamido
 phosphine ligands with ruthenium.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5583
_journal_page_last               5589
_journal_paper_doi               10.1039/c6dt00214e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C20 H38 N2 O P Ru'
_chemical_formula_sum            'C20 H38 N2 O P Ru'
_chemical_formula_weight         454.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/cc1khdbs
_audit_creation_date             2014-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-12-29 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.025(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6117(8)
_cell_length_b                   11.6787(10)
_cell_length_c                   10.5243(10)
_cell_measurement_reflns_used    8834
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.066
_cell_measurement_theta_min      2.711
_cell_volume                     1102.72(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11859
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         2.073
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0569 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.8914.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.7398P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2486
_reflns_number_total             2769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00214e2.cif
_cod_data_source_block           mf997
_cod_depositor_comments          'Adding full bibliography for 7038429.cif.'
_cod_database_code               7038429
_shelxl_version_number           2012-9
_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
 C12-C13
 1.54 with sigma of 0.01
 C14-C15
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C15)
Uanis(C11B) = Uanis(C11)
Uanis(C9B) = Uanis(C11B)
Uanis(C10B) = Uanis(C9B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
 Fixed Sof: C5(0.5) H5A(0.5) H5B(0.5) C4(0.5) H4A(0.5) H4B(0.5) N1(0.5)
 C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C12(0.5) H12A(0.5)
 H12B(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) H15C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H50(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C12(H12A,H12B), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14)
6.c Idealised Me refined as rotating group:
 C9B(H9BA,H9BB,H9BC), C10B(H10A,H10B,H10C), C11B(H11A,H11B,H11C), C9(H9A,H9B,
 H9C), C10(H10D,H10E,H10F), C11(H11D,H11E,H11F), C13(H13A,H13B,H13C), C15(H15A,
 H15B,H15C)
;
_olex2_submission_original_sample_id {[NNP]PBut}RuH(CO)
_olex2_submission_special_instructions 'No special instructions were received'