Experimental and Theoretical Investigation for the Level of Conjugation in Carbazole-Based Precursors and Their Mono-, Di-, and Polynuclear Pt(II) Complexes.
Al-Balushi, Rayya A; Haque, Ashanul; Jayapal, Maharaja; Al-Suti, Mohammed K; Husband, John; Khan, Muhammad S.; Koentjoro, Olivia F.; Molloy, Kieran C.; Skelton, Jonathan M.; Raithby, Paul R.; Inorganic chemistry 55 (2016) 6465–6480; doi:10.1021/acs.inorgchem.6b00523

data_4347722
_publ_section_title
;
 Experimental and Theoretical Investigation for the Level of Conjugation
 in Carbazole-Based Precursors and Their Mono-, Di-, and Polynuclear
 Pt(II) Complexes.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6465
_journal_page_last               6480
_journal_paper_doi               10.1021/acs.inorgchem.6b00523
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C52 H70 N2 P2 Pt'
_chemical_formula_sum            'C52 H70 N2 P2 Pt'
_chemical_formula_weight         980.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                78.149(3)
_cell_angle_beta                 81.742(3)
_cell_angle_gamma                78.372(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5643(3)
_cell_length_b                   10.5536(4)
_cell_length_c                   11.9787(4)
_cell_measurement_reflns_used    8045
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.7390
_cell_measurement_theta_min      3.5120
_cell_volume                     1152.43(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1986 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_details
;
  1 omega  -99.00  -34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.5323 -179.0000  -30.0000 65

  2 omega  -16.00   85.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7041   57.0000  -30.0000 101

  3 omega  -61.00   40.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7041  -57.0000 -180.0000 101

  4 omega  -98.00  -32.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.5323  179.0000 -150.0000 66

  5 omega  -13.00   43.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7041   37.0000  -90.0000 56

  6 omega  -16.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7041   57.0000  150.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0145726000
_diffrn_orient_matrix_UB_12      0.0604835000
_diffrn_orient_matrix_UB_13      0.0083724000
_diffrn_orient_matrix_UB_21      0.0118956000
_diffrn_orient_matrix_UB_22      0.0205949000
_diffrn_orient_matrix_UB_23      -0.0602559000
_diffrn_orient_matrix_UB_31      -0.0737898000
_diffrn_orient_matrix_UB_32      0.0280583000
_diffrn_orient_matrix_UB_33      -0.0013628000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14717
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5584
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                5473
_reflns_number_total             5584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00523_si_001.cif
_cod_data_source_block           p15prr230
_cod_database_code               4347722
_chemical_oxdiff_formula         'C52 H70 N2 P2 Pt'
_chemical_oxdiff_usercomment     'Rayya - Sarah 1st crystal'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C20A, C20B}
3. Restrained distances
 C28B-C29B = C28A-C29A
 1.5 with sigma of 0.02
 C27-C28B
 1.5 with sigma of 0.02
 C27-C28A
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C20A \\sim C20B \\sim C21A \\sim C21B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C29B \\sim C28A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C29A \\sim C28B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C20A) = Uanis(C20B)
5. Others
 Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(H27C)=Sof(H27D)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C28B)=
 Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(H27A)=Sof(H27B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C28A)=
 Sof(H28A)=Sof(H28B)=FVAR(2)
 Fixed Sof: H19A(0.5) H19B(0.5) H19C(0.5) H19D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C19(H19C,H19D), C20A(H20A,H20B), C20B(H20C,
 H20D), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B),
 C27(H27A,H27B), C27(H27C,H27D), C28A(H28A,H28B), C28B(H28C,H28D)
6.b Aromatic/amide H refined with riding coordinates:
 N17(H17), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15)
6.c Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C25(H25A,H25B,H25C), C29A(H29A,
 H29B,H29C), C29B(H29D,H29E,H29F)
;
_olex2_date_sample_data_collection 2015-11-18
_olex2_exptl_crystal_mounting_method
'Mounted in fomblin oil and cooled with an Oxford Diffraction Cryojet'
_olex2_submission_original_sample_id p15prr230
_olex2_submission_special_instructions 'No special instructions were received'