Proton-switchable vapochromic behaviour of a platinum(ii)-carboxy-terpyridine complex.
Kobayashi, Atsushi; Oizumi, Shiori; Shigeta, Yasuhiro; Yoshida, Masaki; Kato, Masako; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17485–17494; doi:10.1039/c6dt03189g

data_7040908
_publ_section_title
;
 Proton-switchable vapochromic behaviour of a
 platinum(ii)-carboxy-terpyridine complex.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17485
_journal_page_last               17494
_journal_paper_doi               10.1039/c6dt03189g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C16 H13 Cl2 N3 O3 Pt'
_chemical_formula_sum            'C16 H13 Cl2 N3 O3 Pt'
_chemical_formula_weight         561.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-09-03 deposited with the CCDC.
2016-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                69.55(4)
_cell_angle_beta                 80.84(4)
_cell_angle_gamma                69.53(3)
_cell_formula_units_Z            2
_cell_length_a                   7.463(6)
_cell_length_b                   9.743(6)
_cell_length_c                   13.044(10)
_cell_measurement_reflns_used    3060
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.02
_cell_volume                     831.8(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68900
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7132
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        24.419
_diffrn_reflns_theta_max         27.343
_diffrn_reflns_theta_min         3.016
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             532.00
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.003
_refine_diff_density_max         2.78
_refine_diff_density_min         -3.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4010
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3608
_reflns_number_total             4010
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6dt03189g2.cif
_cod_data_source_block           1HCl-H2O
_cod_depositor_comments
'Adding full bibliography for 7040907--7040908.cif.'
_cod_database_code               7040908
_shelxl_res_file
;
TITL ohizumi-1
CELL  0.68900 7.46300 9.74300 13.04400 69.55000 80.84000 69.53000
ZERR  2 0.00600 0.00600 0.01000 0.04000 0.04000 0.03000
LATT 1
SFAC C H CL N O PT
UNIT 32 26 4 6 6 2
L.S. 20
FMAP 2
PLAN -25
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -173.0
ACTA
SIZE 0.100 0.010 0.003
WGHT    0.059800
FVAR       0.45308
PT1   6    1.140687    0.319883    0.494897    11.00000    0.00691    0.00763 =
         0.00814   -0.00261   -0.00074   -0.00376
CL1   3    1.357167    0.337440    0.593988    11.00000    0.01112    0.01657 =
         0.01423   -0.00469   -0.00242   -0.00595
CL2   3    0.306955    0.294438    0.001652    11.00000    0.01880    0.01572 =
         0.01070    0.00133   -0.00532   -0.01039
O1    5    0.470659    0.172875    0.281445    11.00000    0.01743    0.02454 =
         0.01443   -0.00637   -0.00071   -0.01591
O2    5    0.579799    0.325270    0.129355    11.00000    0.01951    0.01734 =
         0.01002   -0.00204   -0.00563   -0.01277
AFIX  83
H2A   2    0.497662    0.313453    0.098906    11.00000   -1.20000
AFIX   0
O3    5    1.293267    0.001424    0.944530    11.00000    0.02777    0.03096 =
         0.04494   -0.01744   -0.00848   -0.00961
N1    4    1.031993    0.169969    0.617157    11.00000    0.01262    0.00974 =
         0.00823   -0.00358    0.00219   -0.00549
N2    4    0.960713    0.301834    0.411097    11.00000    0.00664    0.01359 =
         0.01048   -0.00645   -0.00269   -0.00208
N3    4    1.190875    0.463707    0.346767    11.00000    0.01355    0.00618 =
         0.00732   -0.00252    0.00374   -0.00497
C1    1    1.078446    0.106528    0.722695    11.00000    0.01130    0.00848 =
         0.01078   -0.00127   -0.00325   -0.00383
AFIX  43
H1    2    1.177259    0.127924    0.745972    11.00000   -1.20000
AFIX   0
C2    1    0.985013    0.010098    0.798755    11.00000    0.01637    0.01289 =
         0.01200   -0.00464   -0.00076   -0.00384
AFIX  43
H2    2    1.018554   -0.031934    0.873260    11.00000   -1.20000
AFIX   0
C3    1    0.842262   -0.024619    0.765383    11.00000    0.01533    0.01114 =
         0.01604    0.00112    0.00045   -0.00664
AFIX  43
H3    2    0.778750   -0.091285    0.816424    11.00000   -1.20000
AFIX   0
C4    1    0.794506    0.039705    0.656530    11.00000    0.01744    0.00882 =
         0.01203   -0.00467    0.00033   -0.00605
AFIX  43
H4    2    0.696647    0.018692    0.631995    11.00000   -1.20000
AFIX   0
C5    1    0.891454    0.135217    0.583810    11.00000    0.01384    0.00973 =
         0.01215   -0.00422   -0.00520   -0.00357
C6    1    0.852108    0.210754    0.465632    11.00000    0.00864    0.00255 =
         0.01315    0.00047   -0.00002   -0.00307
C7    1    0.724377    0.193772    0.407395    11.00000    0.00927    0.00859 =
         0.01783   -0.00683   -0.00068   -0.00415
AFIX  43
H7    2    0.646966    0.129779    0.443035    11.00000   -1.20000
AFIX   0
C8    1    0.713259    0.273430    0.295153    11.00000    0.01104    0.00653 =
         0.01580   -0.00463   -0.00418   -0.00064
C9    1    0.826446    0.369560    0.241195    11.00000    0.01280    0.01175 =
         0.01084   -0.00479   -0.00162   -0.00324
AFIX  43
H9    2    0.817235    0.424396    0.165023    11.00000   -1.20000
AFIX   0
C10   1    0.952265    0.381149    0.303706    11.00000    0.01013    0.00802 =
         0.01343   -0.00615    0.00042   -0.00504
C11   1    1.083841    0.477460    0.265829    11.00000    0.01115    0.00390 =
         0.01257   -0.00284    0.00091   -0.00284
C12   1    1.099771    0.570002    0.158968    11.00000    0.01098    0.01363 =
         0.01538   -0.00256   -0.00235   -0.00657
AFIX  43
H12   2    1.023996    0.577746    0.103928    11.00000   -1.20000
AFIX   0
C13   1    1.230529    0.651847    0.134207    11.00000    0.01349    0.01197 =
         0.01223   -0.00365    0.00656   -0.00655
AFIX  43
H13   2    1.244429    0.716063    0.061425    11.00000   -1.20000
AFIX   0
C14   1    1.338562    0.639848    0.214358    11.00000    0.01329    0.01214 =
         0.01722   -0.00659    0.00273   -0.00987
AFIX  43
H14   2    1.427787    0.695037    0.197706    11.00000   -1.20000
AFIX   0
C15   1    1.315618    0.544849    0.321477    11.00000    0.00826    0.01183 =
         0.01406   -0.00554   -0.00219   -0.00242
AFIX  43
H15   2    1.389185    0.537273    0.377494    11.00000   -1.20000
AFIX   0
C16   1    0.574601    0.250659    0.234851    11.00000    0.01156    0.01292 =
         0.01318   -0.00680   -0.00082   -0.00332
HKLF 4
 
REM  ohizumi-1
REM R1 =  0.0351 for    3608 Fo > 4sig(Fo)  and  0.0397 for all    4010 data
REM    226 parameters refined using      0 restraints
 
END  
     
WGHT      0.0591      0.0000 

REM Instructions for potential hydrogen bonds
HTAB O2 Cl2
HTAB C1 Cl1
HTAB C1 O3
HTAB C2 O3
EQIV $1 -x+1, -y, -z+1
HTAB C4 O1_$1
EQIV $2 -x+1, -y+1, -z
HTAB C9 Cl2_$2
HTAB C12 Cl2_$2
HTAB C15 Cl1
EQIV $3 -x+3, -y+1, -z+1
HTAB C15 Cl1_$3

REM Highest difference peak  2.782,  deepest hole -3.333,  1-sigma level  0.264
Q1    1   1.2640  0.2191  0.5156  11.00000  0.05    2.78
Q2    1   1.0096  0.4193  0.4799  11.00000  0.05    2.66
Q3    1   1.1283  0.4401  0.4182  11.00000  0.05    2.26
Q4    1   0.5809  0.0397  0.5165  11.00000  0.05    2.06
Q5    1   1.0356  0.3232  0.4448  11.00000  0.05    1.97
Q6    1   1.2573  0.3217  0.5471  11.00000  0.05    1.91
Q7    1   1.1498  0.1971  0.5729  11.00000  0.05    1.89
Q8    1   1.0064  0.3009  0.5249  11.00000  0.05    1.61
Q9    1   1.3581  0.2397  0.4759  11.00000  0.05    1.44
Q10   1   1.0000  0.5000  0.5000  10.50000  0.05    1.35
Q11   1   1.2758  0.3444  0.4689  11.00000  0.05    1.32
Q12   1   1.2454  0.2807  0.4194  11.00000  0.05    1.31
Q13   1   1.0405  0.3577  0.5802  11.00000  0.05    1.20
Q14   1   1.1101  0.4603  0.4980  11.00000  0.05    1.19
Q15   1   1.1498  0.5531  0.4837  11.00000  0.05    1.13
Q16   1   1.1019  0.5158  0.5344  11.00000  0.05    1.11
Q17   1   1.0085  0.5265  0.4194  11.00000  0.05    1.07
Q18   1   1.3779  0.3048  0.3850  11.00000  0.05    1.03
Q19   1   1.2763  0.1277  0.5817  11.00000  0.05    1.00
Q20   1   1.2936  0.2073  0.5929  11.00000  0.05    1.00
Q21   1   1.2754  0.1483  0.5023  11.00000  0.05    0.92
Q22   1   0.5342  0.4010  0.3196  11.00000  0.05    0.88
Q23   1   0.8916  0.3786  0.4558  11.00000  0.05    0.87
Q24   1   1.3133  0.3740  0.3965  11.00000  0.05    0.84
Q25   1   1.4028  0.0644  0.5024  11.00000  0.05    0.84
;