Base assisted C-C coupling between carbonyl and polypyridyl ligands in a Ru-NADH-type carbonyl complex.
Ghosh, Debashis; Fukushima, Takashi; Kobayashi, Katsuaki; Sen, Susan; Kitagawa, Susumu; Kato, Tatsuhisa; Tanaka, Koji; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4373–4381; doi:10.1039/c7dt00312a

data_7042256
_publ_section_title
;
 Base assisted C-C coupling between carbonyl and polypyridyl ligands in a
 Ru-NADH-type carbonyl complex.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4373
_journal_page_last               4381
_journal_paper_doi               10.1039/c7dt00312a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C33 H21 Cl N6 O6.5 Ru'
_chemical_formula_weight         742.08
_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
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2016-11-16 deposited with the CCDC.
2017-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.226(5)
_cell_angle_beta                 98.860(8)
_cell_angle_gamma                97.136(7)
_cell_formula_units_Z            2
_cell_length_a                   8.4666(11)
_cell_length_b                   11.6275(14)
_cell_length_c                   16.1049(19)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.0447
_cell_measurement_theta_min      2.4543
_cell_volume                     1554.0(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12223
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.561
_exptl_absorpt_coefficient_mu    0.649
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       Block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0687P)^2^+2.2893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5862
_reflns_number_total             6747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00312a2.cif
_cod_data_source_block           RutpyCOb_a
_cod_depositor_comments
'Adding full bibliography for 7042254--7042257.cif.'
_cod_original_formula_sum        'C33 H21 Cl N6 O6.50 Ru'
_cod_database_code               7042256
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              34169