A hybrid terpyridine-based bis(diphenylphosphino)amine ligand, terpy-C6H4N(PPh2)2: synthesis, coordination chemistry and photoluminescence studies.
Naik, Susmita; Kumar, Saurabh; Mague, Joel T.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18434–18437; doi:10.1039/c6dt03440c

data_7041050
_publ_section_title
;
 A hybrid terpyridine-based bis(diphenylphosphino)amine ligand,
 terpy-C6H4N(PPh2)2: synthesis, coordination chemistry and
 photoluminescence studies.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18434
_journal_page_last               18437
_journal_paper_doi               10.1039/c6dt03440c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C45 H34 Au2 Cl2 N4 P2, 2(C7 H8), C H2 Cl2'
_chemical_formula_sum            'C60 H52 Au2 Cl4 N4 P2'
_chemical_formula_weight         1426.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-21 deposited with the CCDC.
2016-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                98.626(3)
_cell_angle_beta                 92.793(3)
_cell_angle_gamma                97.092(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9034(6)
_cell_length_b                   13.0595(6)
_cell_length_c                   16.7151(6)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      3.00
_cell_volume                     2757.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37844
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.163
_exptl_absorpt_coefficient_mu    5.610
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         9681
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+8.3312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8670
_reflns_number_total             9681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03440c2.cif
_cod_data_source_block           Compound-4
_cod_depositor_comments
'Adding full bibliography for 7041047--7041050.cif.'
_cod_database_code               7041050
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.534
_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. Restrained distances
 Cl5-C47 \\sim Cl3-C47 \\sim Cl4-C46 \\sim Cl3-C46
 with sigma of 0.02
 N3A-C11A \\sim N3B-C11B
 with sigma of 0.02
 N3A-C15A \\sim N3B-C15B
 with sigma of 0.02
 C14A-C13 \\sim C14B-C13
 with sigma of 0.02
 C12-C11A \\sim C12-C11B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C49A) = Uiso(C49B)
Uanis(N3B) = Uanis(N3A)
Uanis(C15B) = Uanis(C15A)
Uanis(C14B) = Uanis(C14A)
Uiso(C58C) = Uiso(C60A)
Uiso(C47) = Uiso(C46)
Uiso(C11A) = Uiso(C11B)
Uiso(C56A) = Uiso(C57B)
4. Others
 Fixed Sof: Au1A(0.98) Cl2A(0.98) N3B(0.3) C11B(0.3) C14B(0.3) H14B(0.3)
 C15B(0.3) H15B(0.3) C49A(0.7) C53A(0.7) H53A(0.7) C52B(0.7) H52B(0.7)
 C51B(0.7) H51B(0.7) C50B(0.7) H50B(0.7) H50A(0.7) H50C(0.3) C48A(0.7)
 H48A(0.7) H48B(0.7) H48C(0.7) C54A(0.3) H54A(0.3) C49B(0.3) C48B(0.3)
 H48D(0.3) H48E(0.3) H48F(0.3) C51A(0.3) H51A(0.3) C53B(0.3) H53B(0.3)
 C52A(0.3) H52A(0.3) N3A(0.7) C15A(0.7) H15A(0.7) C14A(0.7) H14A(0.7)
 Au1B(0.02) Cl2B(0.02) Cl5(0.55) Cl4(0.45) C46(0.45) H46A(0.45) H46B(0.45)
 C56B(0.34) C57B(0.34) H57B(0.34) C61A(0.34) H61A(0.34) C58C(0.34) H58C(0.34)
 C60B(0.34) H60B(0.34) C61B(0.34) H61B(0.34) C56C(0.33) C61C(0.33) H61C(0.33)
 C60C(0.33) H60C(0.33) C59C(0.33) H59C(0.33) C60A(0.33) H60A(0.33) C57C(0.33)
 H57C(0.33) C55A(0.33) H55G(0.33) H55H(0.33) H55I(0.33) C56A(0.33) C58B(0.33)
 H58B(0.33) C59B(0.33) H59B(0.33) C59A(0.33) H59A(0.33) C58A(0.33) H58A(0.33)
 C57A(0.33) H57A(0.33) C47(0.55) H47A(0.55) H47B(0.55) C11A(0.7) C55B(0.33)
 H55D(0.33) H55E(0.33) H55F(0.33) C55C(0.34) H55A(0.34) H55B(0.34) H55C(0.34)
5.a Riding coordinates:
 C13(H13), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C47(H47A,H47B)
5.c Me refined with riding coordinates:
 C48B(H48D,H48E,H48F), C55A(H55G,H55H,H55I), C55B(H55D,H55E,H55F), C55C(H55A,
 H55B,H55C)
5.d Aromatic/amide H refined with riding coordinates:
 C20(H20), C7(H7), C21(H21), C18(H18), C30(H30), C17(H17), C29(H29), C32(H32),
 C33(H33), C9(H9), C43(H43), C27(H27), C23(H23), C39(H39), C36(H36), C1(H1),
 C2(H2), C24(H24), C37(H37), C26(H26), C25(H25), C38(H38), C14B(H14B),
 C15B(H15B), C41(H41), C31(H31), C3(H3), C35(H35), C42(H42), C4(H4), C45(H45),
 C44(H44), C53A(H53A), C52B(H52B), C51B(H51B), C50B(H50B), C50A(H50A),
 C50A(H50C), C54A(H54A), C51A(H51A), C53B(H53B), C52A(H52A), C15A(H15A),
 C14A(H14A), C57B(H57B), C61A(H61A), C58C(H58C), C60B(H60B), C61B(H61B),
 C61C(H61C), C60C(H60C), C59C(H59C), C60A(H60A), C57C(H57C), C58B(H58B),
 C59B(H59B), C59A(H59A), C58A(H58A), C57A(H57A)
5.e Fitted hexagon refined as free rotating group:
 C49A(C53A,C52B,C51B,C50B,C50A), C56B(C57B,C61A,C58C,C60B,C61B), C56C(C61C,
 C60C,C59C,C60A,C57C), C56A(C58B,C59B,C59A,C58A,C57A)
5.f Idealised Me refined as rotating group:
 C48A(H48A,H48B,H48C)
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_shelx_res_checksum              54794
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'