Effect of positional isomerism on the spectroelectrochemical response of 3,6-bis(2-pyridyl)-diketopyrrolopyrrolate bridged bis(carbonylhydridoruthenium) compounds.
Hazari, Arijit Singha; Ghosh, Prabir; Beyer, Katharina; Schwederski, Brigitte; Kaim, Wolfgang; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14078–14084; doi:10.1039/c8dt02806k

data_7047569
_publ_section_title
;
 Effect of positional isomerism on the spectroelectrochemical response of
 3,6-bis(2-pyridyl)-diketopyrrolopyrrolate bridged
 bis(carbonylhydridoruthenium) compounds.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14078
_journal_page_last               14084
_journal_paper_doi               10.1039/c8dt02806k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C90 H70 N4 O4 P4 Ru2'
_chemical_formula_sum            'C90 H70 N4 O4 P4 Ru2'
_chemical_formula_weight         1597.52
_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   mixed
_audit_creation_date             2018-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-13 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                101.756(2)
_cell_angle_beta                 104.220(2)
_cell_angle_gamma                101.333(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5994(3)
_cell_length_b                   12.0532(4)
_cell_length_c                   16.8855(4)
_cell_measurement_reflns_used    8859
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9800
_cell_measurement_theta_min      1.9230
_cell_volume                     1976.97(11)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20723
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.346
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       needle
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.055
_refine_diff_density_max         2.234
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6960
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0273P)^2^+6.2864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5408
_reflns_number_total             6960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02806k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7047568--7047569.cif.'
_cod_original_cell_volume        1976.97(10)
_cod_database_code               7047569
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 HA-Ru1
 1.5 with sigma of 0.02
 Ru1-H
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C45) = Uanis(C45A)
Uanis(O2) = Uanis(O2A)
4. Others
 Sof(C45A)=Sof(O2A)=Sof(HA)=1-FVAR(1)
 Sof(C45)=Sof(O2)=Sof(H)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C20(H20), C6(H6), C42(H42), C19(H19), C37(H37), C16(H16), C5(H5),
 C43(H43), C44(H44), C10(H10), C7(H7), C8(H8), C22(H22), C11(H11), C35(H35),
 C41(H41), C26(H26), C14(H14), C40(H40), C18(H18), C25(H25), C24(H24), C12(H12),
  C13(H13), C23(H23), C34(H34), C17(H17), C36(H36), C32(H32), C28(H28),
 C31(H31), C30(H30), C29(H29)
;
_shelx_res_checksum              52918
_shelx_fab_checksum              68261
_olex2_submission_special_instructions 'No special instructions were received'