Alkyne substituted mononuclear photocatalysts based on [RuCl(bpy)(tpy)](.).
Davidson, Ross J.; Wilson, Lucy E.; Duckworth, Andrew R.; Yufit, Dmitry S.; Beeby, Andrew; Low, Paul J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11368–11379; doi:10.1039/c5dt01278c

data_7034851
_publ_section_title
;
 Alkyne substituted mononuclear photocatalysts based on
 [RuCl(bpy)(tpy)](.).
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11368
_journal_page_last               11379
_journal_paper_doi               10.1039/c5dt01278c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C34 H25 Cl N5 Ru, F6 P, C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C40 H38 Cl F6 N6 O P Ru'
_chemical_formula_weight         900.25
_chemical_name_systematic
;
 ? 
;
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-12
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2015-02-02 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                74.903(3)
_cell_angle_beta                 81.701(3)
_cell_angle_gamma                82.307(3)
_cell_formula_units_Z            4
_cell_length_a                   12.0142(14)
_cell_length_b                   13.6517(16)
_cell_length_c                   24.769(3)
_cell_measurement_reflns_used    6948
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.29
_cell_volume                     3861.4(8)
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            66133
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         1.55
_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    0.587
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0589 before and 0.0384 after correction.
The Ratio of minimum to maximum transmission is 0.3864.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic greenish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.887
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         21526
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+6.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                14837
_reflns_number_total             21526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01278c2.cif
_cod_data_source_block           13srv090
_cod_depositor_comments
'Adding full bibliography for 7034850--7034852.cif.'
_cod_database_code               7034851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H23A of C23A, H13A of C13A, H1A of C1A, H9A of C9A, H14A of C14A, H34A of
  C34A, H26A of C26A, H27 of C27, H4 of C4, H3 of C3, H2 of C2, H1 of C1, H31A
  of C31A, H28A of C28A, H2A of C2A, {H5SA,H5SB} of C5S, H33A of C33A, H22A of
  C22A, H13 of C13, H12 of C12, H9 of C9, H7 of C7, H31 of C31, H4A of C4A, H3A
  of C3A, H20A of C20A, H7A of C7A, H25 of C25, H26 of C26, H22 of C22, H27A of
  C27A, H25A of C25A, H28 of C28, H15A of C15A, {H7SA,H7SB} of C7S, H19A of
  C19A, H12A of C12A, H23 of C23, H20 of C20, {H11A,H11B} of C11S, H34 of C34,
  H32A of C32A, {H9SA,H9SB} of C9S, H32 of C32, H33 of C33, H19 of C19, H15 of
  C15, H14 of C14
 At 1.5 times of:
  {H6SA,H6SB,H6SC} of C6S, {H4SD,H4SE,H4SF} of C4S, {H24D,H24E,H24F} of C24,
  {H8SA,H8SB,H8SC} of C8S, {H2SA,H2SB,H2SC} of C2SA, {H4SA,H4SB,H4SC} of C4SA,
  {H2SD,H2SE,H2SF} of C2SB, {H24A,H24B,H24C} of C24A, {H12B,H12C,H12D} of C12S,
  {H10A,H10B,H10C} of C10S
2. Restrained distances
 P2-F9B ~ P2-F10B ~ P2-F10A ~ P2-F11B ~ P2-F11A ~ P2-F8B ~ P2-F8A ~ P2-F9A ~
 P1B-F2B ~ P1B-F2A ~ P1B-F3A ~ P1B-F3B ~ P1B-F4A ~ P1B-F4B ~ P1B-F5B ~ P1B-F5A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C8S) ~ Ueq, Uanis(C7S) ~ Ueq, Uanis(O1) ~ Ueq, Uanis(C5S) ~ Ueq, 
Uanis(C6S) ~ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: P1A(0.5) P1B(0.5) F2A(0.5) F2B(0.5) F3A(0.5) F3B(0.5) F4A(0.5)
 F4B(0.5) F5A(0.5) F5B(0.5) F6A(0.5) F6B(0.5) F8A(0.5) F8B(0.5) F9A(0.5)
 F9B(0.5) F10A(0.5) F10B(0.5) F11A(0.5) F11B(0.5) N1SB(0.5) C1SB(0.5) C2SB(0.5)
 H2SD(0.5) H2SE(0.5) H2SF(0.5) N2S(0.5) C4S(0.5) H4SD(0.5) H4SE(0.5) H4SF(0.5)
 C3S(0.5) N3S(0.5) C4SA(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5) C3SA(0.5) C2SA(0.5)
 H2SA(0.5) H2SB(0.5) H2SC(0.5) N1SA(0.5) C1SA(0.5)
5.a Riding coordinates:
 C4S(H4SD,H4SE,H4SF)
5.b Secondary CH2 refined with riding coordinates:
 C5S(H5SA,H5SB), C7S(H7SA,H7SB), C11S(H11A,H11B), C9S(H9SA,H9SB)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C1A(H1A), C2A(H2A),
 C3A(H3A), C4A(H4A), C7A(H7A), C9A(H9A), C12A(H12A), C13A(H13A), C14A(H14A),
 C15A(H15A), C19A(H19A), C20A(H20A), C22A(H22A), C23A(H23A), C25A(H25A),
 C26A(H26A), C27A(H27A), C28A(H28A), C31A(H31A), C32A(H32A), C33A(H33A),
 C34A(H34A)
5.d Idealised Me refined as rotating group:
 C24(H24D,H24E,H24F), C24A(H24A,H24B,H24C), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,
 H8SC), C10S(H10A,H10B,H10C), C12S(H12B,H12C,H12D), C2SB(H2SD,H2SE,H2SF),
 C4SA(H4SA,H4SB,H4SC), C2SA(H2SA,H2SB,H2SC)
;