Extremely low-frequency phonon material and its temperature- and photo-induced switching effects
Yoshida, Takaya; Nakabayashi, Koji; Tokoro, Hiroko; Yoshikiyo, Marie; Namai, Asuka; Imoto, Kenta; Chiba, Kouji; Ohkoshi, Shin-ichi; Chemical Science  (2020) –; doi:10.1039/D0SC02605K

data_1558862
_publ_section_title
;
 Extremely low-frequency phonon material and its temperature- and
 photo-induced switching effects
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02605K
_journal_year                    2020
_chemical_formula_moiety         'C20 H8 Co N12 Rb W'
_chemical_formula_sum            'C20 H8 Co N12 Rb W'
_chemical_formula_weight         744.63
_chemical_name_common            RbCo[W(CN)8](3CNpy)2_LT_phase
_chemical_name_systematic        RbCoW3CNpy_LT_phase
_chemical_properties_physical    Hygroscopic
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-05 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                118.671(8)
_cell_angle_beta                 100.497(7)
_cell_angle_gamma                90.100(6)
_cell_formula_units_Z            2
_cell_length_a                   7.2253(14)
_cell_length_b                   13.340(3)
_cell_length_c                   13.839(3)
_cell_measurement_reflns_used    7584
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      55.000
_cell_measurement_theta_min      5.980
_cell_volume                     1144.6(4)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Rapid Auto'
_diffrn_measurement_method       omega
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.989
_exptl_absorpt_coefficient_mu    7.895
_exptl_absorpt_correction_T_max  0.8331
_exptl_absorpt_correction_T_min  0.2958
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.024
_refine_diff_density_max         3.355
_refine_diff_density_min         -5.698
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5234
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.1105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0012P)^2^+48.6694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4267
_reflns_number_total             5234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02605k4.cif
_cod_data_source_block           shelxl
_cod_database_code               1558862
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.296
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 W1-C7A
 2.15 with sigma of 0.05
 W1-C7B
 2.15 with sigma of 0.05
 C7A-N7A
 1.14 with sigma of 0.05
 C7B-N7B
 1.14 with sigma of 0.05
 C6B-N6B
 1.14 with sigma of 0.05
 W1-C6B
 2.15 with sigma of 0.05
 C20L-C16L
 1.45 with sigma of 0.05
 C20-C16
 1.45 with sigma of 0.05
 C16L-C20L
 1.45 with sigma of 0.05
 C10-C14
 1.45 with sigma of 0.05
 C10L-C14L
 1.45 with sigma of 0.05
 C20-N12
 1.13 with sigma of 0.05
 C20L-N12L
 1.13 with sigma of 0.05
 C14-N10
 1.13 with sigma of 0.05
 C14L-N10L
 1.13 with sigma of 0.05
 N5B-C5B
 1.14 with sigma of 0.05
 W1-C5B
 2.15 with sigma of 0.05
3. Restrained planarity
 N9, N10, C9, C10, C11, C12, C13, C14
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C18L \\sim C19L: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uiso(C15L) = Uiso(C15)
Uiso(N11L) = Uiso(N11)
Uiso(N9L) = Uiso(N9)
Uiso(C9L) = Uiso(C9)
5. Others
 Fixed Sof: Rb1A(0.5) N5A(0.5) N6A(0.5) N7A(0.5) N8A(0.5) N9(0.5) N10(0.5)
 N11(0.5) N12(0.5) C5A(0.5) C6A(0.5) C7A(0.5) C9(0.5) H9(0.5) C10(0.5) C11(0.5)
 H11(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C14(0.5) C15(0.5) H15(0.5)
 C16(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5)
 Rb1B(0.5) N5B(0.5) N6B(0.5) N7B(0.5) N8B(0.5) N9L(0.5) N10L(0.5) N11L(0.5)
 N12L(0.5) C5B(0.5) C6B(0.5) C7B(0.5) C9L(0.5) H9L(0.5) C10L(0.5) C11L(0.5)
 H11L(0.5) C12L(0.5) H12L(0.5) C13L(0.5) H13L(0.5) C14L(0.5) C15L(0.5)
 H15L(0.5) C16L(0.5) C17L(0.5) H17L(0.5) C18L(0.5) H18L(0.5) C19L(0.5)
 H19L(0.5) C20L(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C12(H12), C13(H13), C15(H15), C17(H17), C18(H18), C19(H19),
 C9L(H9L), C11L(H11L), C12L(H12L), C13L(H13L), C15L(H15L), C17L(H17L),
 C18L(H18L), C19L(H19L)
;
_shelx_res_checksum              69159
_olex2_submission_special_instructions 'No special instructions were received'