New molecular architectures containing low-valent cluster centres with di- and trimetalated 2-vinylpyrazine ligands: synthesis and molecular structures of Ru5(CO)15(μ5-C4H2N2CHCH)(μ-H)2 and Ru8(CO)24(μ7-C4H2N2CHC)(μ-H)3
Hossain, Md. Monir; Akter, Nahid; Ghosh, Shishir; Nesterov, Vladimir N.; Richmond, Michael G.; Hogarth, Graeme; Kabir, Shariff E.; RSC Advances 9 (2019) 21025–; doi:10.1039/C9RA03841H

data_7233024
_publ_section_title
;
 New molecular architectures containing low-valent cluster centres with
 di- and trimetalated 2-vinylpyrazine ligands: synthesis and molecular
 structures of Ru5(CO)15(\m5-C4H2N2CH&#xE001;CH)(\m-H)2 and
 Ru8(CO)24(\m7-C4H2N2CH&#xE001;C)(\m-H)3
;
_journal_issue                   36
_journal_name_full               'RSC Advances'
_journal_page_first              21025
_journal_paper_doi               10.1039/C9RA03841H
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C21 H6 N2 O15 Ru5'
_chemical_formula_sum            'C21 H6 N2 O15 Ru5'
_chemical_formula_weight         1031.63
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-08 deposited with the CCDC.    2019-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                75.588(2)
_cell_angle_beta                 79.665(2)
_cell_angle_gamma                77.224(2)
_cell_formula_units_Z            4
_cell_length_a                   9.2594(5)
_cell_length_b                   14.0086(8)
_cell_length_c                   23.9807(14)
_cell_measurement_reflns_used    8324
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.27
_cell_volume                     2912.5(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            151823
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.361
_diffrn_reflns_theta_min         2.275
_exptl_absorpt_coefficient_mu    2.606
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0973 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.6995.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.353
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5216
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00129(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         14508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+1.6791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0298
_refine_ls_wR_factor_ref         0.0305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13586
_reflns_number_total             14508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03841h2.cif
_cod_data_source_block           ap3ol
_cod_database_code               7233024
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.422
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C17(H17), C37(H37), C38(H38)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C40(H40), C42(H42)
;
_olex2_submission_special_instructions 'No special instructions were received'