Reaction of carbonyl trinuclear clusters with 2,5-bis(2-thienyl)-1-phenyl-phosphole as a ligand: a new pathway to ruthenacyclopentadiene and cyclopentadienone ruthenium complexes
Otero, Yomaira; Peña, Deisy; Lescop, Christophe; Ávila, Edward; Arce, Alejandro; Hissler, Muriel; Réau, Regis; Machado, Rubén; New Journal of Chemistry 42 (2018) 12234–; doi:10.1039/C8NJ01442F

data_7057543
_publ_section_title
;
 Reaction of carbonyl trinuclear clusters with
 2,5-bis(2-thienyl)-1-phenyl-phosphole as a ligand: a new pathway to
 ruthenacyclopentadiene and cyclopentadienone ruthenium complexes
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12234
_journal_paper_doi               10.1039/C8NJ01442F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C43 H33 O5 P Ru2 S4'
_chemical_formula_sum            'C43 H33 O5 P Ru2 S4'
_chemical_formula_weight         991.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9476(5)
_cell_length_b                   18.3390(9)
_cell_length_c                   19.9476(9)
_cell_measurement_reflns_used    8134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.22
_cell_volume                     3940.1(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.9958
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by SAINT Bruker-AXS'
_diffrn_orient_matrix_UB_11      -0.41612E-2
_diffrn_orient_matrix_UB_12      -0.496756E-1
_diffrn_orient_matrix_UB_13      0.201428E-1
_diffrn_orient_matrix_UB_21      -0.526547E-1
_diffrn_orient_matrix_UB_22      0.196867E-1
_diffrn_orient_matrix_UB_23      0.319373E-1
_diffrn_orient_matrix_UB_31      -0.763561E-1
_diffrn_orient_matrix_UB_32      -0.108686E-1
_diffrn_orient_matrix_UB_33      -0.342147E-1
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26445
_diffrn_reflns_theta_full        26.4359
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick,G.M.(2002). SADABS, Bruker AXS Inc.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.6707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1985.1407
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.6416
_refine_diff_density_min         -0.6134
_refine_diff_density_rms         0.1052
_refine_ls_d_res_high            0.7982
_refine_ls_d_res_low             8.6520
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0594
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    94
_refine_ls_number_parameters     545
_refine_ls_number_reflns         8075
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.0440
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.0463
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+9.2597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7681
_reflns_number_total             8075
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8nj01442f2.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 7057540--7057543.cif.'
_cod_database_code               7057543
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C13A, S2A, C14A, C15A, C16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13B, S2B, C14B, C15B, C16B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S4A, C35B, C36A, C37A, C38A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S4B, C35B, C36B, C37B, C38B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30A, S3A, C31A, C32A, C33A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30B, S3B, C31B, C32B, C33B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C13A \\sim S2A \\sim C14A \\sim C15A \\sim C16A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C13B \\sim S2B \\sim C14B \\sim C15B \\sim C16B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
S4A \\sim C35A \\sim C36A \\sim C37A \\sim C38A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
S4B \\sim C35A \\sim C36B \\sim C37B \\sim C38B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C30A \\sim S3A \\sim C31A \\sim C32A \\sim C33A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C30B \\sim S3B \\sim C31B \\sim C32B \\sim C33B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(S2A) = Uanis(S2B)
Uanis(C13A) = Uanis(C13B)
Uanis(C14A) = Uanis(C14B)
Uanis(C15A) = Uanis(C15B)
Uanis(C16A) = Uanis(C16B)
Uanis(S4A) = Uanis(S4B)
Uanis(C35A) = Uanis(C35B)
Uanis(C36A) = Uanis(C36B)
Uanis(C37A) = Uanis(C37B)
Uanis(C38A) = Uanis(C38B)
Uanis(S3A) = Uanis(S3B)
Uanis(C30A) = Uanis(C30B)
Uanis(C31A) = Uanis(C31B)
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
4. Same fragment restrains
{C13B, S2B, C14B, C15B, C16B} sigma for 1-2: 0.02, 1-3: 0.04
{C13A, S2A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C13A, S2A, C14A, C15A, C16A}
{S3B, C30B, C31B, C32B, C33B} sigma for 1-2: 0.02, 1-3: 0.04
{S3A, C30A, C31A, C32A, C33A} sigma for 1-2: 0.02, 1-3: 0.04
as
{S3A, C30A, C31A, C32A, C33A}
{S4A, C35B, C36A, C37A, C38A} sigma for 1-2: 0.02, 1-3: 0.04
{S4B, C35B, C36B, C37B, C38B} sigma for 1-2: 0.02, 1-3: 0.04
as
{S4A, C35A, C36A, C37A, C38A}
5. Others
 Sof(S3A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=1-FVAR(1)
 Sof(S3B)=Sof(C30B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=
 Sof(H33B)=FVAR(1)
 Sof(S4A)=Sof(C35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=
 Sof(H38A)=1-FVAR(2)
 Sof(S4B)=Sof(C35B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=Sof(H37B)=Sof(C38B)=
 Sof(H38B)=FVAR(2)
 Sof(C13B)=Sof(S2B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=
 Sof(H16B)=1-FVAR(3)
 Sof(C13A)=Sof(S2A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16A)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C24(H24a,H24b), C25(H25a,
 H25b), C26(H26a,H26b), C27(H27a,H27b)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C14A(H14A), C15A(H15A), C16A(H16A), C14B(H14B),
 C15B(H15B), C16B(H16B), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C31A(H31A), C32A(H32A), C33A(H33A), C31B(H31B), C32B(H32B), C33B(H33B),
 C36A(H36A), C37A(H37A), C38A(H38A), C36B(H36B), C37B(H37B), C38B(H38B)
;
_olex2_submission_special_instructions 'No special instructions were received'