Cyclometalated Platinum(II) Complexes of 1,3-Bis(1-n-butylpyrazol-3-yl)benzenes: Synthesis, Characterization, Electrochemical, Photophysical, and Gelation Behavior Studies.
Ai, Yeye; Li, Yongguang; Ma, Huiqing; Su, Cheng-Yong; Yam, Vivian Wing-Wah; Inorganic chemistry 55 (2016) 11920–11929; doi:10.1021/acs.inorgchem.6b02033

data_4349175
_publ_section_title
;
 Cyclometalated Platinum(II) Complexes of
 1,3-Bis(1-n-butylpyrazol-3-yl)benzenes: Synthesis, Characterization,
 Electrochemical, Photophysical, and Gelation Behavior Studies.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11920
_journal_page_last               11929
_journal_paper_doi               10.1021/acs.inorgchem.6b02033
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H25 Cl N4 Pt'
_chemical_formula_sum            'C21 H25 Cl N3 Pt'
_chemical_formula_weight         549.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.32728(15)
_cell_length_b                   11.17560(16)
_cell_length_c                   16.8866(2)
_cell_measurement_reflns_used    3713
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8000
_cell_measurement_theta_min      3.9360
_cell_volume                     1948.94(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5072
_diffrn_reflns_theta_full        73.77
_diffrn_reflns_theta_max         73.77
_diffrn_reflns_theta_min         4.74
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.790
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                3310
_reflns_number_total             3363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02033_si_002.cif
_cod_data_source_block           COMPLEX_1
_cod_original_cell_volume        1948.95(5)
_cod_database_code               4349175
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.964(12) 0.036(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C13(H13A,H13B), C18(H18A,H18B), C19(H19A,
 H19B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C1(H1), C12(H12), C2(H2), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'