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_7233026
_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         'C30 H6 N2 O24 Ru8'
_chemical_formula_sum            'C30 H6 N2 O24 Ru8'
_chemical_formula_weight         1586.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-08 deposited with the CCDC.    2019-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.089(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3141(12)
_cell_length_b                   31.916(4)
_cell_length_c                   13.0093(14)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2989
_cell_measurement_theta_min      2.3773
_cell_volume                     4216.2(9)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0307
_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       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.489
_exptl_absorpt_coefficient_mu    2.873
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0908 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.7958.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'intense orange'
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.000083(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+28.2021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7958
_reflns_number_total             9295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03841h2.cif
_cod_data_source_block           my17better
_cod_original_cell_volume        4216.2(8)
_cod_database_code               7233026
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.611
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 HB-Ru7 = HB-Ru8
 1.8 with sigma of 0.01
 HA-Ru4 = HA-Ru8
 1.8 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C26(H26)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30)
;
_shelx_res_checksum              24965
_olex2_submission_special_instructions 'No special instructions were received'