Coordinating Tectons: Bimetallic Complexes from Bipyridyl Terminated Group 8 Alkynyl Complexes
Koutsantonis, George A.; Low, Paul J.; Mackenzie, Campbell F. R.; Skelton, Brian W.; Yufit, Dmitry S.; Organometallics 33 (2014) 4911–; doi:10.1021/om500172r

data_4084207
_publ_section_title
;
 Coordinating Tectons: Bimetallic Complexes from Bipyridyl Terminated
 Group 8 Alkynyl Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4911
_journal_paper_doi               10.1021/om500172r
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C51 H46 Cl N2 O3 P2 Re Ru, 0.5(C H Cl3)'
_chemical_formula_sum            'C51.5 H46.5 Cl2.5 N2 O3 P2 Re Ru'
_chemical_formula_weight         1179.24
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.02.11 svn.r2872 for OlexSys, GUI svn.r4756)
;
_cell_angle_alpha                114.681(3)
_cell_angle_beta                 109.232(4)
_cell_angle_gamma                91.551(4)
_cell_formula_units_Z            2
_cell_length_a                   13.582(5)
_cell_length_b                   13.773(5)
_cell_length_c                   15.307(6)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.87
_cell_volume                     2411.0(16)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device       ' 'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.688900
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27191
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.02
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    2.812
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1532 before and 0.0351 after correction.
The Ratio of minimum to maximum transmission is 0.7888.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.0049(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         12905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0575P)^2^+3.9586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                11253
_reflns_number_total             12905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500172r_si_001.cif
_cod_data_source_block           5_n12srv231
_cod_original_formula_sum        'C51.50 H46.50 Cl2.50 N2 O3 P2 Re Ru'
_cod_database_code               4084207
_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. Others
 Fixed Sof: Cl2(0.5) Cl3(0.5) Cl4(0.5) C1S(0.5) H1S(0.5) CNT1(0)
3.a Everything fixed:
 CNT1
3.b Ternary CH refined with riding coordinates:
 C1S(H1S)
3.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B)
3.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), 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)
3.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C)
;