Reversible Pyrrole-Based Proton Storage/Release in Ruthenium(II) Complexes
Zhang, Zheng-Hao; He, Piao; Kang, Shi-Rui; Liu, Chao; Yi, Xiao-Yi; Chemical Communications  (2019) –; doi:10.1039/C9CC08288C

data_7124435
_publ_section_title
;
 Reversible Pyrrole-Based Proton Storage/Release in Ruthenium(II)
 Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC08288C
_journal_year                    2019
_chemical_formula_moiety         'C29 H23 Br N6 Ru, C F3 O3 S, C F3 O3 S0.59'
_chemical_formula_sum            'C31 H23 Br F6 N6 O6 Ru S1.76'
_chemical_formula_weight         926.88
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-17 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.331(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5132(6)
_cell_length_b                   10.8824(3)
_cell_length_c                   18.0933(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      2.20
_cell_volume                     3443.49(18)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52177
_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         26.435
_diffrn_reflns_theta_min         2.204
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0565 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.8428.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7067
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0926P)^2^+9.2623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4807
_reflns_number_total             7067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08288c2.cif
_cod_data_source_block           1
_cod_database_code               7124435
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 S1A, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C30, F5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C30, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C30, S2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
F3 \\sim F3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F2 \\sim F2A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F1 \\sim F1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F4 \\sim F4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F5 \\sim F5A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F6 \\sim F6A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(F3A)=Sof(F2A)=Sof(F1A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C27(H27), C28(H28), C29(H29)
;
_shelx_res_checksum              18021
_olex2_submission_special_instructions 'No special instructions were received'