Reversible single-crystal-to-single-crystal photoisomerization of a silver(i) macropolyhedral borane
Avdeeva, Varvara V.; Buzin, Mikhail I.; Malinina, Elena A.; Kuznetsov, Nikolay T.; Vologzhanina, Anna V.; CrystEngComm 17 (2015) 8870–; doi:10.1039/C5CE00859J

data_1520078
_publ_section_title
;
 Reversible single-crystal-to-single-crystal photoisomerization of a
 silver(i) macropolyhedral borane
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8870
_journal_paper_doi               10.1039/C5CE00859J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         '2(C54 H45 Ag P3), B20 H18'
_chemical_formula_sum            'C108 H108 Ag2 B20 P6'
_chemical_formula_weight         2023.70
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Light-sensitive
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-12 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 131.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9900(8)
_cell_length_b                   25.1550(14)
_cell_length_c                   21.7332(14)
_cell_measurement_reflns_used    5661
_cell_measurement_temperature    353
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.25
_cell_volume                     5299.6(6)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      353
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            80819
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.375
_diffrn_reflns_theta_min         1.923
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.1591
_exptl_absorpt_correction_T_min  0.1074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0957 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.6750.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_recrystallization_method
'solid state reaction by heating of the iso-isomer'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         18906
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+1.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10904
_reflns_number_total             18906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00859j2.cif
_cod_data_source_block           1ht
_cod_depositor_comments
'Adding full bibliography for 1520076--1520078.cif.'
_cod_database_code               1520078
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All B(H,H) groups, All C(H) groups
2. Restrained distances
 B7-B3A
 1.7 with sigma of 0.02
 B4-B3A
 1.7 with sigma of 0.02
 B10-B3A
 1.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B3A \\sim B3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
B6 \\sim B6A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
B1 \\sim B1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
B2A \\sim B2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
B10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: B1(0.75) H1(0.75) B2(0.75) B3(0.75) H3A(0.75) H5A(0.75) H5B(0.25)
 B6(0.75) H6A(0.75) H7A(0.75) H7B(0.25) H9A(0.75) H9B(0.25) H10B(0.25)
 H10A(0.75) B2A(0.25) H2A(0.25) B6A(0.25) H6AA(0.25) B3A(0.25) H3AA(0.25)
 B1A(0.25)
 Fixed Uiso: B2A(0.07)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
5.b Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3A), B4(H4A), B5(H5A), B5(H5B), B6(H6A), B7(H7A), B7(H7B),
 B8(H8A), B9(H9A), B9(H9B), B10(H10B), B10(H10A), B2A(H2A), B6A(H6AA), B3A(H3AA)
;
_shelx_res_checksum              34989