Noninnocence of the deprotonated 1,2-bis((1<i>H</i>-pyrrol-2-yl)methylene)hydrazine bridge in diruthenium frameworks - a function of co-ligands.
Kumari, Maya; Bera, Sudip Kumar; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9891–9903; doi:10.1039/d1dt01488a

data_7707670
_publ_section_title
;
 Noninnocence of the deprotonated
 1,2-bis((1<i>H</i>-pyrrol-2-yl)methylene)hydrazine bridge in diruthenium
 frameworks - a function of co-ligands.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9891
_journal_page_last               9903
_journal_paper_doi               10.1039/d1dt01488a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C30 H36 N4 O8 Ru2'
_chemical_formula_sum            'C30 H36 N4 O8 Ru2'
_chemical_formula_weight         781.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                100.6410(10)
_cell_angle_beta                 91.2890(10)
_cell_angle_gamma                104.4110(10)
_cell_formula_units_Z            4
_cell_length_a                   9.6955(5)
_cell_length_b                   19.0317(9)
_cell_length_c                   19.4285(6)
_cell_measurement_reflns_used    6851
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.17
_cell_volume                     3403.6(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20712
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.176
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4623
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1393 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.6200.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             1582
_refine_diff_density_max         1.989
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         11114
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0668
_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^)+(0.1187P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8646
_reflns_number_total             11114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01488a2.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
Adding full bibliography for 7707670--7707674.cif.

2024-10-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C57 H72 N15 O12 Ru4'
_cod_original_formula_weight         1563.57
_cod_original_formula_moiety         '2(C30 H36 N4 O8 Ru2)'
_cod_original_formula_units_Z            2
_cod_database_code               7707670
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C48) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C13(H13), C18(H18), C5(H5), C3(H3), C23(H23), C28(H28),
 C10(H10), C9(H9), C8(H8), C6(H6), C43(H43), C48(H48), C36(H36), C53(H53),
 C58(H58), C40(H40), C39(H39), C38(H38), C35(H35), C33(H33), C32(H32), C31(H31)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C30(H30A,
 H30B,H30C), C45(H45A,H45B,H45C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C),
 C46(H46A,H46B,H46C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C60(H60A,H60B,
 H60C), C56(H56A,H56B,H56C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53878
_shelx_hkl_checksum              77203
_shelx_fab_checksum              81233
_olex2_submission_special_instructions 'No special instructions were received'