pH-driven optical changes of platinum(II) complexes having carboxy-appended salophen ligands
Fjii, Shun; Yagi, Hajime; Kawaguchi, Tomohiro; Ishikawa, Mitsuru; Izumiyama, Naoki; Nakaya, Manabu; Dalton Transactions  (2023) –; doi:10.1039/D3DT00956D

data_7713416
_publ_section_title
;
 pH-driven optical changes of platinum(II) complexes having
 carboxy-appended salophen ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00956D
_journal_year                    2023
_chemical_formula_moiety         'C21 H13 N2 O4 Pt, H2 O'
_chemical_formula_sum            'C21 H15 N2 O5 Pt'
_chemical_formula_weight         570.44
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-10 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.9491(5)
_cell_length_b                   19.9491(5)
_cell_length_c                   8.8324(3)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.36
_cell_volume                     3044.08(15)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            36523
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         3.120
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.948
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1115 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8006.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1793
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.728
_refine_ls_shift/su_mean         0.068
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+17.6614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1378
_reflns_number_total             1793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00956d10.cif
_cod_data_source_block           hexa_a
_cod_original_cell_volume        3044.08(18)
_cod_database_code               7713416
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.606
_shelx_estimated_absorpt_t_min   0.352
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained planarity
 C8, C9, C10, C11, O3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C10 \\sim C11 \\sim O3: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O3(0.5) C11(0.5) O5(0.25) H5A(0.25) H5B(0.25) O4(0.25) H4A(0.25)
 H4B(0.25) O2(0.5) H2A(0.5)
5.a Free rotating group:
 O5(H5A,H5B), O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C2(H2), C3(H3), C4(H4), C5(H5)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              9420
_olex2_submission_special_instructions 'No special instructions were received'