#------------------------------------------------------------------------------
#$Date: 2017-07-01 04:20:22 +0200 (Sat 01 de Jul de 2017) $
#$Revision: 198301 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/35/7043500.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7043500
loop_
_publ_author_name
'Zhang, Yuzhen'
'Hauke, Cory E.'
'Crawley, Matthew R.'
'Schurr, Bradley E.'
'Fulong, Cressa Ria P.'
'Cook, Timothy'
_publ_section_title
;
 Increasing phosphorescent quantum yields and lifetimes of
 platinum-alkynyl complexes with extended conjugation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01817G
_journal_year                    2017
_chemical_formula_moiety         'C26 H38 N2 P2 Pt'
_chemical_formula_sum            'C26 H38 N2 P2 Pt'
_chemical_formula_weight         635.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-26 deposited with the CCDC.
2017-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4820(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8056(4)
_cell_length_b                   11.2252(5)
_cell_length_c                   14.0390(7)
_cell_measurement_reflns_used    5670
_cell_measurement_temperature    106.05
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      3.02
_cell_volume                     1330.66(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      106.05
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10280
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.036
_diffrn_reflns_theta_min         3.019
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.408
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0757 before and 0.0349 after correction. The Ratio of minimum to maximum transmission is 0.7103. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       Block
_exptl_crystal_F_000             632
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slow evaporation from CH2Cl2/Hexanes'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0050P)²+1.1050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3038
_reflns_number_total             4154
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01817g3.cif
_cod_data_source_block           mrc_yz_289_0m
_cod_database_code               7043500
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.563
_shelx_estimated_absorpt_t_min   0.313
_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. Rigid bond restraints
 C5, C6, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C8(H8A,H8B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), C5(H5)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pt1 Pt 0.0000 0.5000 0.0000 0.01049(4) Uani 1 2 d S T P
P1 P 0.24772(7) 0.44521(6) 0.09737(5) 0.01236(12) Uani 1 1 d . . .
C2 C -0.1081(3) 0.5795(2) 0.19062(19) 0.0158(5) Uani 1 1 d . . .
C3 C -0.1625(3) 0.6130(2) 0.27356(19) 0.0148(5) Uani 1 1 d . . .
C1 C -0.0660(3) 0.5508(2) 0.11905(19) 0.0158(5) Uani 1 1 d . . .
C12 C 0.3915(3) 0.5602(2) 0.0921(2) 0.0179(5) Uani 1 1 d . . .
H12A H 0.4997 0.5305 0.1244 0.022 Uiso 1 1 calc R . .
H12B H 0.3837 0.5781 0.0219 0.022 Uiso 1 1 calc R . .
C8 C 0.2647(3) 0.4272(2) 0.22889(18) 0.0171(5) Uani 1 1 d . . .
H8A H 0.2269 0.5013 0.2529 0.021 Uiso 1 1 calc R . .
H8B H 0.1928 0.3622 0.2360 0.021 Uiso 1 1 calc R . .
C10 C 0.3266(3) 0.3090(2) 0.0595(2) 0.0193(6) Uani 1 1 d . . .
H10A H 0.3328 0.3186 -0.0094 0.023 Uiso 1 1 calc R . .
H10B H 0.4354 0.2961 0.1030 0.023 Uiso 1 1 calc R . .
C11 C 0.2269(4) 0.2004(2) 0.0644(2) 0.0304(7) Uani 1 1 d . . .
H11A H 0.1174 0.2145 0.0247 0.046 Uiso 1 1 calc GR . .
H11B H 0.2293 0.1855 0.1336 0.046 Uiso 1 1 calc GR . .
H11C H 0.2695 0.1311 0.0382 0.046 Uiso 1 1 calc GR . .
C9 C 0.4303(3) 0.3996(3) 0.2964(2) 0.0259(6) Uani 1 1 d . . .
H9A H 0.5058 0.4579 0.2846 0.039 Uiso 1 1 calc GR . .
H9B H 0.4617 0.3194 0.2819 0.039 Uiso 1 1 calc GR . .
H9C H 0.4295 0.4039 0.3660 0.039 Uiso 1 1 calc GR . .
C13 C 0.3629(3) 0.6742(2) 0.1441(2) 0.0241(6) Uani 1 1 d . . .
H13A H 0.2499 0.6940 0.1226 0.036 Uiso 1 1 calc GR . .
H13B H 0.4239 0.7396 0.1268 0.036 Uiso 1 1 calc GR . .
H13C H 0.3966 0.6620 0.2162 0.036 Uiso 1 1 calc GR . .
C4 C -0.2493(3) 0.7172(2) 0.2740(2) 0.0247(6) Uani 1 1 d . . .
H4 H -0.2692 0.7708 0.2195 0.030 Uiso 1 1 calc R . .
C7 C -0.1330(3) 0.5418(3) 0.3587(2) 0.0255(6) Uani 1 1 d . . .
H7 H -0.0696 0.4727 0.3616 0.031 Uiso 1 1 calc R . .
C6 C -0.2745(4) 0.6628(4) 0.4307(3) 0.0509(11) Uani 1 1 d . U .
H6 H -0.3175 0.6791 0.4842 0.061 Uiso 1 1 calc R . .
N1 N -0.1876(3) 0.5644(3) 0.43596(19) 0.0436(7) Uani 1 1 d . U .
C5 C -0.3056(3) 0.7413(3) 0.3536(3) 0.0410(9) Uani 1 1 d . U .
H5 H -0.3651 0.8116 0.3550 0.049 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Pt1 P1 180.0 3_565 .
C1 Pt1 P1 91.78(7) . .
C1 Pt1 P1 88.22(7) . 3_565
C1 Pt1 P1 91.78(7) 3_565 3_565
C1 Pt1 P1 88.22(7) 3_565 .
C1 Pt1 C1 180.00(12) 3_565 .
C12 P1 Pt1 109.75(8) . .
C8 P1 Pt1 115.01(8) . .
C8 P1 C12 105.13(12) . .
C10 P1 Pt1 115.22(9) . .
C10 P1 C12 104.85(12) . .
C10 P1 C8 105.95(12) . .
C1 C2 C3 178.3(3) . .
C4 C3 C2 122.2(2) . .
C4 C3 C7 116.3(3) . .
C7 C3 C2 121.5(2) . .
C2 C1 Pt1 178.7(2) . .
C13 C12 P1 111.30(19) . .
C9 C8 P1 116.15(19) . .
C11 C10 P1 112.85(19) . .
C5 C4 C3 119.5(3) . .
N1 C7 C3 124.5(3) . .
N1 C6 C5 124.3(3) . .
C7 N1 C6 116.5(3) . .
C6 C5 C4 118.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 P1 2.3050(6) 3_565
Pt1 P1 2.3050(6) .
Pt1 C1 2.002(3) 3_565
Pt1 C1 2.002(3) .
P1 C12 1.824(3) .
P1 C8 1.821(3) .
P1 C10 1.820(3) .
C2 C3 1.429(4) .
C2 C1 1.209(4) .
C3 C4 1.398(3) .
C3 C7 1.400(4) .
C12 C13 1.528(4) .
C8 C9 1.528(3) .
C10 C11 1.515(4) .
C4 C5 1.373(4) .
C7 N1 1.329(4) .
C6 N1 1.334(5) .
C6 C5 1.362(5) .
