Pressure-induced non-innocence in bis(1,2-dionedioximato)Pt(ii) complexes: an experimental and theoretical study of their insulator-metal transitions.
Benjamin, Helen; Richardson, Jonathan G.; Moggach, Stephen A.; Afanasjevs, Sergejs; Warren, Lisette; Warren, Mark R.; Allan, David R.; Morrison, Carole A.; Kamenev, Konstantin V.; Robertson, Neil; Physical chemistry chemical physics : PCCP 22 (2020) 6677–6689; doi:10.1039/c9cp06749c

data_7240075
_publ_section_title
;
 Pressure-induced non-innocence in bis(1,2-dionedioximato)Pt(ii)
 complexes: an experimental and theoretical study of their insulator-metal
 transitions.
;
_journal_issue                   12
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              6677
_journal_page_last               6689
_journal_paper_doi               10.1039/c9cp06749c
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 N4 O4 Pt1'
_chemical_formula_sum            'C12 H10 N4 O4 Pt'
_chemical_formula_weight         469.33
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-09
_audit_creation_method           CRYSTALS_ver_14.61_build_6720
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5805(9)
_cell_length_b                   20.129(16)
_cell_length_c                   5.8077(9)
_cell_measurement_reflns_used    581
_cell_measurement_temperature    293
_cell_measurement_theta_max      18
_cell_measurement_theta_min      2
_cell_volume                     1120.0(9)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         2380000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.300
_diffrn_measured_fraction_theta_max 0.282
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1131
_diffrn_reflns_theta_full        13.239
_diffrn_reflns_theta_max         17.652
_diffrn_reflns_theta_min         1.609
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.554
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         5.01
_refine_diff_density_min         -2.13
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1635
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         178
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.0000224
_refine_ls_shift/su_mean         0.0000048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 228. -156. 205. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1883
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.1883
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              0
_reflns_number_gt                178
_reflns_number_total             180
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      62.33
_oxford_refine_ls_r_factor_ref   0.0834
_oxford_refine_ls_scale          0.1605(9)
_oxford_reflns_number_all        178
_oxford_structure_analysis_title 'final in Ibam'
_cod_data_source_file            c9cp06749c2.cif
_cod_data_source_block           PtBQD_238
_cod_depositor_comments
'Adding full bibliography for 7240068--7240076.cif.'
_cod_original_sg_symbol_Hall     '-I 2 2c '
_cod_original_sg_symbol_H-M      'I b a m '
_cod_original_formula_sum        'C12 H10 N4 O4 Pt1'
_cod_database_code               7240075
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)