Transforming PPh<sub>3</sub> into bidentate phosphine ligands at Ru-Zn heterobimetallic complexes.
O'Leary, Niall; Miloserdov, Fedor M.; Mahon, Mary F.; Whittlesey, Michael K.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14000–14009; doi:10.1039/c9dt03106e

data_7700938
_publ_section_title
;
 Transforming PPh<sub>3</sub> into bidentate phosphine ligands at Ru-Zn
 heterobimetallic complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14000
_journal_page_last               14009
_journal_paper_doi               10.1039/c9dt03106e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C63 H49 P3 Ru Zn'
_chemical_formula_sum            'C65 H53 O0.5 P3 Ru Zn'
_chemical_formula_weight         1101.42
_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
_audit_creation_date             2019-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-01 deposited with the CCDC.    2019-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                79.451(2)
_cell_angle_beta                 81.396(2)
_cell_angle_gamma                80.252(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8687(2)
_cell_length_b                   12.1871(3)
_cell_length_c                   20.5157(5)
_cell_measurement_reflns_used    17970
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9930
_cell_measurement_theta_min      4.1390
_cell_volume                     2613.16(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30751
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.107
_diffrn_reflns_theta_min         4.015
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         10334
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0326P)^2^+1.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9537
_reflns_number_total             10334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03106e2.cif
_cod_data_source_block           s19mkw5
_cod_depositor_comments
'Adding full bibliography for 7700936--7700938.cif.'
_cod_original_cell_volume        2613.17(11)
_cod_original_formula_sum        'C65 H53 O0.50 P3 Ru Zn'
_cod_database_code               7700938
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'red block crystals'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-C52A \\sim P1-C51 \\sim P1-C58A \\sim P1-C58
 with sigma of 0.005
 C34-C35 \\sim C34-C35A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C36-C37 \\sim C36A-C37
 with sigma of 0.02
 C36-C37A \\sim C36A-C37A
 with sigma of 0.02
 P2-C34 \\sim P2-C34A
 with sigma of 0.02
 C34-C35 \\sim C34A-C35
 with sigma of 0.02
 C34-C39 \\sim C34A-C39
 with sigma of 0.02
 C34-C39A \\sim C34A-C39A
 with sigma of 0.02
 C34-C35A \\sim C34A-C35A
 with sigma of 0.02
 C36A-C35A \\sim C36-C35 \\sim C37-C36 \\sim C37A-C36A \\sim C38A-C37A \\sim
C38-C37 \\sim C39A-C38A ~
 C39-C38 \\sim C39-C34 \\sim C35-C34 \\sim C35A-C34A
 with sigma of 0.005
3. Restrained planarity
 C34, C35, C36, C37, C38, C39
 with sigma of 0.1
 C34A, C35A, C36A, C37A, C38A, C39A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
C0AA \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C57A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C40A \\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim C45A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C36 \\sim C36A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01
Uanis(C34) = Uanis(C34A)
5. Others
 Fixed Sof: Zn1(0.53) P3(0.53) C0AA(0.53) H0AA(0.53) C1(0.53) H1A(0.53)
 H1B(0.53) H1C(0.53) C34(0.53) C35(0.53) H35(0.53) C36(0.53) H36(0.53)
 C37(0.53) H37(0.53) C38(0.53) H38(0.53) C39(0.53) C40(0.53) C41(0.53)
 H41(0.53) C42(0.53) H42(0.53) C43(0.53) H43(0.53) C44(0.53) H44(0.53)
 C45(0.53) C46(0.53) H46(0.53) C47(0.53) H47(0.53) C48(0.53) H48(0.53)
 C49(0.53) H49(0.53) C50(0.53) H50(0.53) C51(0.53) C52(0.53) H52(0.53)
 C53(0.53) H53(0.53) C54(0.53) H54(0.53) C55(0.53) H55(0.53) C56(0.53)
 H56(0.53) C58(0.53) C59(0.53) H59(0.53) C60(0.53) H60(0.53) C61(0.53)
 H61(0.53) C62(0.53) H62(0.53) C63(0.53) H63(0.53) Zn1A(0.47) P3A(0.47)
 C1A(0.47) H1AA(0.47) H1AB(0.47) H1AC(0.47) C34A(0.47) C35A(0.47) H35A(0.47)
 C36A(0.47) H36A(0.47) C37A(0.47) H37A(0.47) C38A(0.47) H38A(0.47) C39A(0.47)
 C40A(0.47) C41A(0.47) H41A(0.47) C42A(0.47) H42A(0.47) C43A(0.47) H43A(0.47)
 C44A(0.47) H44A(0.47) C45A(0.47) H45A(0.47) C46A(0.47) C47A(0.47) H47A(0.47)
 C48A(0.47) H48A(0.47) C49A(0.47) H49A(0.47) C50A(0.47) H50A(0.47) C51A(0.47)
 H51A(0.47) C52A(0.47) C53A(0.47) H53A(0.47) C54A(0.47) H54A(0.47) C55A(0.47)
 H55A(0.47) C56A(0.47) H56A(0.47) C57A(0.47) H57A(0.47) C58A(0.47) C59A(0.47)
 H59A(0.47) C60A(0.47) H60A(0.47) C61A(0.47) H61A(0.47) C62A(0.47) H62A(0.47)
 C63A(0.47) H63A(0.47)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C0AA(H0AA), C35(H35),
 C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C41A(H41A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C47A(H47A), C48A(H48A), C49A(H49A),
 C50A(H50A), C51A(H51A), C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A),
 C57A(H57A), C59A(H59A), C60A(H60A), C61A(H61A), C62A(H62A), C63A(H63A)
6.b Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C56), C58(C59,C60,C61,C62,C63), C52A(C53A,C54A,C55A,C56A,
 C57A), C58A(C59A,C60A,C61A,C62A,C63A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;