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_7040907
_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 H17 Cl N3 O5.5 Pt'
_chemical_formula_sum            'C16 H17 Cl N3 O5.5 Pt'
_chemical_formula_weight         569.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                90.0000
_cell_angle_beta                 100.119(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.925(5)
_cell_length_b                   17.917(13)
_cell_length_c                   14.788(11)
_cell_measurement_reflns_used    3393
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      1.75
_cell_volume                     1806(2)
_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      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68900
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16104
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.419
_diffrn_reflns_theta_max         25.837
_diffrn_reflns_theta_min         2.204
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1092.00
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.67
_refine_diff_density_min         -3.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3789
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                2949
_reflns_number_total             3789
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6dt03189g2.cif
_cod_data_source_block           1_3-5H2O
_cod_depositor_comments
'Adding full bibliography for 7040907--7040908.cif.'
_cod_database_code               7040907
_shelxl_res_file
;
TITL 150806oizumi-r
CELL  0.68900 6.92530 17.91690 14.78830 90.00000 100.11930 90.00000
ZERR  4 0.00490 0.01250 0.01090 0.00000 0.01020 0.00000
LATT 1
SYMM .50-X, .50+Y,    -Z
SFAC C H CL N O PT
UNIT 64 68 4 12 22 4
L.S. 50
FMAP 2
PLAN -25
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -99.8
ACTA
SIZE 0.075 0.020 0.010
WGHT    0.075200
FVAR       0.38232
PT1   6    0.778151    0.267307    0.379010    11.00000    0.02049    0.01916 =
         0.02264   -0.00111    0.00272    0.00033
CL1   3    0.768706    0.390453    0.425208    11.00000    0.03885    0.02219 =
         0.03694   -0.00539    0.00619    0.00299
O1    5    0.857981   -0.071859    0.177680    11.00000    0.06489    0.03635 =
         0.06046   -0.01342    0.03493    0.00610
O2    5    0.694254   -0.107652    0.287530    11.00000    0.05473    0.02794 =
         0.04221    0.00198    0.00678   -0.00742
O3    5    0.520840    0.498677    0.044197    10.50000    0.09228    0.04692 =
         0.10744   -0.04612    0.07332   -0.01811
O4    5    0.864021    0.554614    0.015777    11.00000    0.06594    0.03924 =
         0.05438   -0.00379    0.01323   -0.00279
O5    5    0.536959   -0.313910    0.106934    11.00000    0.04429    0.02583 =
         0.04750    0.00785    0.01037   -0.00193
O6    5    0.943215   -0.326675    0.143733    11.00000    0.04165    0.02741 =
         0.03398    0.00238    0.00277    0.00671
O7    5    0.342628   -0.264607    0.141276    10.35000    0.02350    0.09473 =
         0.07322   -0.02900    0.01186   -0.02929
N1    4    0.792285    0.286173    0.244803    11.00000    0.02553    0.02730 =
         0.02100   -0.00234    0.00069    0.00581
N2    4    0.781422    0.163900    0.339520    11.00000    0.01497    0.02994 =
         0.02433   -0.00082   -0.00060    0.00400
N3    4    0.767290    0.216607    0.500253    11.00000    0.02238    0.02648 =
         0.02049   -0.00198   -0.00260   -0.00087
C1    1    0.795428    0.351166    0.202274    11.00000    0.02366    0.02430 =
         0.03365    0.00634    0.00427   -0.00165
AFIX  43
H1    2    0.789073    0.395997    0.235927    11.00000   -1.20000
AFIX   0
C2    1    0.807970    0.355344    0.108338    11.00000    0.03707    0.04100 =
         0.02724    0.01205    0.01083    0.00107
AFIX  43
H2    2    0.806207    0.402478    0.078781    11.00000   -1.20000
AFIX   0
C3    1    0.822522    0.291926    0.060527    11.00000    0.02827    0.04962 =
         0.02373    0.00440    0.00307    0.00096
AFIX  43
H3    2    0.834161    0.294504   -0.002455    11.00000   -1.20000
AFIX   0
C4    1    0.820451    0.221475    0.104225    11.00000    0.02670    0.03513 =
         0.02367    0.00212    0.00297   -0.00156
AFIX  43
H4    2    0.829953    0.176308    0.071646    11.00000   -1.20000
AFIX   0
C5    1    0.804101    0.221151    0.195856    11.00000    0.02050    0.02904 =
         0.02445   -0.00316    0.00810    0.00166
C6    1    0.795959    0.151779    0.250464    11.00000    0.02025    0.02366 =
         0.01953   -0.00206   -0.00477   -0.00342
C7    1    0.798979    0.078442    0.219435    11.00000    0.02463    0.02523 =
         0.03465   -0.00602    0.00634    0.00382
AFIX  43
H5    2    0.811727    0.067709    0.157849    11.00000   -1.20000
AFIX   0
C8    1    0.782630    0.021077    0.281902    11.00000    0.03139    0.01895 =
         0.02967   -0.00710    0.01112   -0.00403
C9    1    0.767924    0.035700    0.372558    11.00000    0.02022    0.02804 =
         0.02559   -0.00089    0.00738   -0.00147
AFIX  43
H6    2    0.756632   -0.003541    0.414516    11.00000   -1.20000
AFIX   0
C10   1    0.770417    0.111591    0.400120    11.00000    0.01199    0.04275 =
         0.01968   -0.00931   -0.00039    0.00015
C11   1    0.766864    0.140205    0.494524    11.00000    0.02765    0.02934 =
         0.02727    0.00361    0.00544    0.00637
C12   1    0.756389    0.096866    0.570068    11.00000    0.03627    0.03125 =
         0.03710    0.00908    0.00828    0.00600
AFIX  43
H7    2    0.757867    0.044006    0.565205    11.00000   -1.20000
AFIX   0
C13   1    0.743834    0.129697    0.652293    11.00000    0.04920    0.03665 =
         0.02247    0.00177    0.01025   -0.00301
AFIX  43
H8    2    0.733528    0.100030    0.704475    11.00000   -1.20000
AFIX   0
C14   1    0.746355    0.206685    0.658385    11.00000    0.03935    0.04314 =
         0.01962   -0.00332    0.00675   -0.00327
AFIX  43
H9    2    0.737949    0.230644    0.714870    11.00000   -1.20000
AFIX   0
C15   1    0.761321    0.248558    0.580942    11.00000    0.02956    0.03125 =
         0.02429   -0.00247    0.00724   -0.00305
AFIX  43
H10   2    0.767464    0.301414    0.585673    11.00000   -1.20000
AFIX   0
C16   1    0.780892   -0.061044    0.246633    11.00000    0.04665    0.01836 =
         0.03116   -0.00020    0.00547    0.00267
HKLF 4
 
REM  150806oizumi-r
REM R1 =  0.0530 for    2949 Fo > 4sig(Fo)  and  0.0711 for all    3789 data
REM    253 parameters refined using      0 restraints
 
END  
     
WGHT      0.0752      0.0000 

REM Instructions for potential hydrogen bonds
HTAB C1 Cl1
HTAB C2 O3
EQIV $1 -x+3/2, y-1/2, -z
HTAB C7 O4_$1
EQIV $2 -x+3/2, y-1/2, -z+1
HTAB C12 Cl1_$2
EQIV $3 -x+1, -y, -z+1
HTAB C14 O7_$3
HTAB C15 Cl1
EQIV $4 -x+3/2, y+1/2, -z+1
HTAB C15 O2_$4

REM Highest difference peak  2.668,  deepest hole -3.191,  1-sigma level  0.289
Q1    1   0.7787  0.1945  0.3790  11.00000  0.05    2.67
Q2    1   0.6069  0.2662  0.3324  11.00000  0.05    2.26
Q3    1   0.7196  0.5097  0.1829  11.00000  0.05    2.15
Q4    1   0.9444  0.2642  0.4226  11.00000  0.05    1.50
Q5    1   0.8021  0.3872  0.3438  11.00000  0.05    1.49
Q6    1   0.9709  0.2702  0.3635  11.00000  0.05    1.17
Q7    1   0.7144  0.2658  0.4413  11.00000  0.05    1.16
Q8    1   0.7478  0.2707  0.2923  11.00000  0.05    1.08
Q9    1   0.4763 -0.3218  0.1438  11.00000  0.05    1.06
Q10   1   1.0073  0.3098  0.3413  11.00000  0.05    1.01
Q11   1   0.5003  0.2373  0.2406  11.00000  0.05    0.99
Q12   1   0.4729 -0.1602  0.1400  11.00000  0.05    0.98
Q13   1   1.1037  0.2939  0.4780  11.00000  0.05    0.98
Q14   1   0.4926 -0.2279  0.1433  11.00000  0.05    0.96
Q15   1   0.8588  0.2695  0.4714  11.00000  0.05    0.95
Q16   1   1.1027  0.2632  0.4678  11.00000  0.05    0.92
Q17   1   0.5070 -0.2028  0.0968  11.00000  0.05    0.88
Q18   1   1.0039  0.4909  0.1938  11.00000  0.05    0.81
Q19   1   0.9522 -0.0089  0.4328  11.00000  0.05    0.78
Q20   1   0.4523  0.2788  0.2826  11.00000  0.05    0.78
Q21   1   0.5297 -0.1438  0.2045  11.00000  0.05    0.77
Q22   1   0.5949  0.0681  0.6796  11.00000  0.05    0.77
Q23   1   0.4336  0.4814  0.0479  11.00000  0.05    0.76
Q24   1   1.0329  0.3077  0.4319  11.00000  0.05    0.76
Q25   1   0.7364  0.2109  0.4520  11.00000  0.05    0.75
;