Bismuth and antimony halometalates containing photoswitchable ruthenium nitrosyl complexes.
Mikhailov, Artem; Korobeynikov, Nikita; Usoltsev, Andrey; Adonin, Sergey A.; Kostin, Gennadiy A.; Schaniel, Dominik; Dalton transactions (Cambridge, England : 2003) 52 (2023) 919–927; doi:10.1039/d2dt03497b

data_7711973
_publ_section_title
;
 Bismuth and antimony halometalates containing photoswitchable ruthenium
 nitrosyl complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              919
_journal_page_last               927
_journal_paper_doi               10.1039/d2dt03497b
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         '3(Bi2 Br9), 4(C20 H20 Br N5 O Ru), 4(H2 O)'
_chemical_formula_sum            'C80 H88 Bi6 Br31 N20 O8 Ru4'
_chemical_formula_weight         5593.07
_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   mixed
_audit_creation_date             2022-12-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                96.349(3)
_cell_angle_beta                 103.183(3)
_cell_angle_gamma                105.167(3)
_cell_formula_units_Z            2
_cell_length_a                   15.1913(13)
_cell_length_b                   17.2926(12)
_cell_length_c                   27.970(3)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      2.32
_cell_volume                     6790.5(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            73912
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.438
_exptl_absorpt_coefficient_mu    17.348
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.8485.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.735
_exptl_crystal_description       block
_exptl_crystal_F_000             5062
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.055
_refine_diff_density_max         3.251
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         25709
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0525
_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^)+123.6990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19789
_reflns_number_total             25709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03497b2.cif
_cod_data_source_block           nk730
_cod_depositor_comments
'Adding full bibliography for 7711973--7711974.cif.'
_cod_original_cell_volume        6790.4(10)
_cod_database_code               7711973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.449
_shelx_estimated_absorpt_t_min   0.449
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br1B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.002
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3. Others
 Sof(Br1A)=1-FVAR(1)
 Sof(Br30)=FVAR(1)
 Sof(Br1B)=1-FVAR(2)
 Sof(Br31)=FVAR(2)
4.a Free rotating group:
 O3(H3A,H3B), O4(H4A,H4B), O2(H2A,H2B), O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C113(H113), C12(H12), C63(H63), C102(H102), C33(H33), C23(H23), C203(H203),
 C153(H153), C161(H161), C143(H143), C192(H192), C111(H111), C43(H43), C32(H32),
  C42(H42), C121(H121), C142(H142), C202(H202), C193(H193), C13(H13),
 C133(H133), C93(H93), C101(H101), C163(H163), C72(H72), C53(H53), C91(H91),
 C22(H22), C123(H123), C62(H62), C103(H103), C92(H92), C52(H52), C174(H174),
 C82(H82), C152(H152), C112(H112), C54(H54), C172(H172), C11(H11), C83(H83),
 C162(H162), C141(H141), C131(H131), C44(H44), C191(H191), C173(H173),
 C182(H182), C73(H73), C201(H201), C151(H151), C154(H154), C24(H24), C171(H171),
  C51(H51), C204(H204), C61(H61), C31(H31), C144(H144), C14(H14), C71(H71),
 C181(H181), C41(H41), C194(H194), C34(H34), C164(H164), C183(H183), C132(H132),
  C81(H81), C184(H184), C122(H122), C134(H134), C114(H114), C64(H64), C74(H74),
 C124(H124), C94(H94), C21(H21), C104(H104), C84(H84)
;
_shelx_res_checksum              85393
_shelx_hkl_checksum              64912
_olex2_submission_special_instructions 'No special instructions were received'