TbCo and Tb0.5Dy0.5Co layered cyanido-bridged frameworks for construction of colorimetric and ratiometric luminescent thermometers
Kumar, Kunal; Chorazy, Szymon; Nakabayashi, Koji; Sato, Hiroyasu; Sieklucka, Barbara; Ohkoshi, Shin-ichi; Journal of Materials Chemistry C 6 (2018) 8372–; doi:10.1039/C8TC01305E

data_7237316
_publ_section_title
;
 TbCo and Tb0.5Dy0.5Co layered cyanido-bridged frameworks for construction
 of colorimetric and ratiometric luminescent thermometers
;
_journal_issue                   31
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              8372
_journal_paper_doi               10.1039/C8TC01305E
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety
'C13.6 H6.4 Co0.8 N6.4 O4 Tb0.8, 2(C1.2 H0.8 Co0.1 N0.8 O0.3 Tb0.1), 0.4(O)'
_chemical_formula_sum            'C16 H8 Co N8 O5 Tb'
_chemical_formula_weight         610.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-13 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.059(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.8969(7)
_cell_length_b                   15.6638(14)
_cell_length_c                   9.6068(10)
_cell_measurement_reflns_used    7100
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.2240
_cell_measurement_theta_min      3.0130
_cell_modulation_dimension       1
_cell_volume                     1014.94(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.40b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.40b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.40b (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50   24.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   24.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50   24.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50   24.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  Rigaku_AFC10_724P_007HF_Mo
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0702999000
_diffrn_orient_matrix_UB_12      0.0312358000
_diffrn_orient_matrix_UB_13      -0.0310594000
_diffrn_orient_matrix_UB_21      0.0772141000
_diffrn_orient_matrix_UB_22      0.0250290000
_diffrn_orient_matrix_UB_23      -0.0176338000
_diffrn_orient_matrix_UB_31      -0.0125483000
_diffrn_orient_matrix_UB_32      -0.0211795000
_diffrn_orient_matrix_UB_33      -0.0664998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.116
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.40b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         24.483
_refine_diff_density_min         -4.900
_refine_diff_density_rms         0.867
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.524
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3174
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.467
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.1365
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3487
_refine_ls_wR_factor_ref         0.3592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2636
_reflns_number_total             3174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc01305e2.cif
_cod_data_source_block           data
_cod_database_code               7237316
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         TbCoC20H20N20O10
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N2A, Tb1}
{N2B, O2}
{N5, O2B}
3. Restrained distances
 C2B-Co1B
 1.87 with sigma of 0.02
 N2B-C2B
 1.16 with sigma of 0.02
 Co1B-C1B
 1.87 with sigma of 0.01
 N1B-C1B
 1.16 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O1A \\sim Tb1A \\sim C2A \\sim C6A \\sim C5A \\sim C4A \\sim C7A \\sim N4A
\\sim C1A \\sim N3A \\sim N2A \\sim O3A \\sim C3A \\sim Co1A \\sim O2A \\sim
N1A: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Co1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
Uiso(N2B) = Uiso(O2)
Uiso(N5) = Uiso(O2B)
Uiso(N2A) = Uiso(Tb1)
Uiso(Co1B) = Uiso(C1B) = Uiso(N1B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Tb1(0.4) Co1(0.4) N3(0.4) O2(0.4) N2(0.4) N1(0.8) N5(0.4) O1(0.8)
 C9(0.8) H9(0.8) O3(0.8) C7(0.8) H7(0.8) C1(0.8) C8(0.8) N6(0.8) C10(0.8)
 H10(0.8) C6(0.8) H6(0.8) C2A(0.05) Tb1A(0.05) O1A(0.1) O3B(0.1) Co1A(0.05)
 C1A(0.05) N4A(0.1) C3A(0.1) H3A(0.1) C4A(0.1) H4A(0.1) C5A(0.1) C6A(0.1)
 H6A(0.1) C7A(0.1) H7A(0.1) N1A(0.1) Tb1B(0.05) O1B(0.1) O3A(0.1) Co1B(0.05)
 C2B(0.05) N3B(0.1) C3B(0.1) H3B(0.1) C4B(0.1) H4B(0.1) C5B(0.1) C6B(0.1)
 H6B(0.1) C7B(0.1) H7B(0.1) N2B(0.05) N4(0.4) N2A(0.05) C1B(0.05) N1B(0.1)
 N4B(0.15) N3A(0.15) O2B(0.05) O2A(0.05)
 Fixed Uiso: C2A(0.001) Tb1A(0.001) O1A(0.001) O3B(0.001) Co1A(0.001)
 C1A(0.001) N4A(0.001) C3A(0.001) C4A(0.001) C5A(0.001) C6A(0.001) C7A(0.001)
 N1A(0.001) Tb1B(0.001) O1B(0.001) O3A(0.001) Co1B(0.001) C2B(0.001) N3B(0.001)
 C3B(0.001) C4B(0.001) C5B(0.001) C6B(0.001) C7B(0.001) C1B(0.001) N1B(0.001)
 N4B(0.001) N3A(0.001) O2A(0.001)
 Fixed X: C1A(0.66748) C1B(-0.301169)
 Fixed Y: C1A(0.37548)
 Fixed Z: C1A(0.47893)
7.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C10(H10), C6(H6), C3A(H3A), C4A(H4A), C6A(H6A), C7A(H7A),
 C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B)
7.b Fitted hexagon refined as free rotating group:
 N4A(C3A,C4A,C5A,C6A,C7A), N3B(C3B,C4B,C5B,C6B,C7B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.827
_oxdiff_exptl_absorpt_empirical_full_min 0.669