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_1520077
_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    Heat-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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-03-12 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 131.7390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9112(9)
_cell_length_b                   25.0981(18)
_cell_length_c                   21.0634(14)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    120
_cell_measurement_theta_max      36.04
_cell_measurement_theta_min      2.26
_cell_volume                     5093.1(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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            91811
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         36.55
_diffrn_reflns_theta_min         1.78
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.2220
_exptl_absorpt_correction_T_min  0.1467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0819 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.6608.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_recrystallization_method
'solid state reaction under UV irradiation of the trans isomer'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         23939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+7.2411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                18152
_reflns_number_total             23939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00859j2.cif
_cod_data_source_block           UV
_cod_depositor_comments
'Adding full bibliography for 1520076--1520078.cif.'
_cod_database_code               1520077
_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. Others
 Fixed Sof: H4A(0.6) H4B(0.4) B1A(0.6) H1A(0.6) B3A(0.6) H3A(0.6) B5A(0.6)
 H5A(0.6) B6A(0.6) H6A(0.6) B7A(0.6) H7A(0.6) B8A(0.6) H8A(0.6) B10A(0.6)
 H10A(0.6) B1B(0.4) H1B(0.4) B3B(0.4) H3B(0.4) B5B(0.4) H5B(0.4) B6B(0.4)
 H6B(0.4) B7B(0.4) H7B(0.4) B8B(0.4) H8B(0.4) B10B(0.4) H10B(0.4)
3.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)
3.b Boron cage BH refined with riding coordinates:
 B4(H4A), B4(H4B), B1A(H1A), B3A(H3A), B5A(H5A), B6A(H6A), B7A(H7A), B8A(H8A),
 B10A(H10A), B1B(H1B), B3B(H3B), B5B(H5B), B6B(H6B), B7B(H7B), B8B(H8B),
 B10B(H10B)
;
_olex2_submission_special_instructions 'No special instructions were received'