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_4349176
_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_formula_moiety         'C28 H29 N5 O2 Pt'
_chemical_formula_sum            'C28 H33 N5 O2 Pt'
_chemical_formula_weight         666.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-20
_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                 109.946(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0990(2)
_cell_length_b                   16.5708(3)
_cell_length_c                   13.1513(2)
_cell_measurement_reflns_used    9343
_cell_measurement_temperature    289.41(10)
_cell_measurement_theta_max      76.0680
_cell_measurement_theta_min      3.5070
_cell_volume                     2478.54(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      289.41(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -65.00   3.00   1.00    1.00    --  -41.20  38.00 -90.00   68
  2  \w    -63.00  31.00   1.00    1.00    --  -41.20  38.00-180.00   94
  3  \w    -40.00  -2.00   1.00    1.00    --  -41.20 125.00-120.00   38
  4  \w     84.00 159.00   1.00    1.00    --  112.00  61.00-180.00   75
  5  \w    101.00 171.00   1.00    1.00    --  112.00 125.00 -90.00   70
  6  \w    119.00 145.00   1.00    1.00    --  112.00 139.00  33.00   26
  7  \w     89.00 115.00   1.00    1.00    --  112.00 139.00  33.00   26
  8  \w     92.00 117.00   1.00    1.00    --  112.00  30.00  60.00   25
  9  \w    132.00 157.00   1.00    1.00    --  112.00  30.00  60.00   25
 10  \w     59.00 106.00   1.00    1.00    --  112.00 -94.00 -30.00   47
 11  \w     94.00 121.00   1.00    1.00    --  112.00-125.00 -30.00   27
 12  \w     56.00  97.00   1.00    1.00    --  112.00 -94.00  90.00   41
 13  \w     63.00 139.00   1.00    1.00    --  112.00 -30.00 120.00   76
 14  \w     47.00 106.00   1.00    1.00    --  112.00 -61.00 -60.00   59
 15  \w     51.00  77.00   1.00    1.00    --  112.00-125.00-180.00   26
 16  \w     85.00 121.00   1.00    1.00    --  112.00-125.00-180.00   36
 17  \w     48.00  97.00   1.00    1.00    --   41.20-125.00 -90.00   49
 18  \w     30.00  96.00   1.00    1.00    --  112.00 -94.00 -60.00   66
 19  \w     98.00 157.00   1.00    1.00    --  112.00 125.00-150.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0086584000
_diffrn_orient_matrix_UB_12      -0.0927689000
_diffrn_orient_matrix_UB_13      0.0059647000
_diffrn_orient_matrix_UB_21      -0.1349550000
_diffrn_orient_matrix_UB_22      -0.0057611000
_diffrn_orient_matrix_UB_23      -0.0357305000
_diffrn_orient_matrix_UB_31      -0.0074254000
_diffrn_orient_matrix_UB_32      -0.0028686000
_diffrn_orient_matrix_UB_33      -0.1192264000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13260
_diffrn_reflns_theta_full        76.03
_diffrn_reflns_theta_max         76.03
_diffrn_reflns_theta_min         4.72
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.402
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.00077(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+1.4436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                4971
_reflns_number_total             5133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02033_si_003.cif
_cod_data_source_block           COMPLEX_5
_cod_original_cell_volume        2478.54(7)
_cod_database_code               4349176
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C19(H19A,
 H19B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C1(H1), C11(H11), C5(H5), C28(H28), C12(H12), C27(H27),
 C25(H25), C6(H6), C24(H24)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.123
_oxdiff_exptl_absorpt_empirical_full_min 0.587