Sensitised lanthanide luminescence using a Ru<sup>II</sup> polypyridyl functionalised dipicolinic acid chelate.
Rajah, Divya; Pfrunder, Michael C.; Chong, Bowie S. K.; Ireland, Alexander R.; Etchells, Isaac M.; Moore, Evan G.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7400–7408; doi:10.1039/d1dt00982f

data_7707361
_publ_section_title
;
 Sensitised lanthanide luminescence using a Ru<sup>II</sup> polypyridyl
 functionalised dipicolinic acid chelate.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7400
_journal_page_last               7408
_journal_paper_doi               10.1039/d1dt00982f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C45 H33 F12 K N7 O4 P2 Ru, F6 P'
_chemical_formula_sum            'C45 H33 F18 K N7 O4 P3 Ru'
_chemical_formula_weight         1310.86
_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             2020-06-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-02-25 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                89.234(5)
_cell_angle_beta                 85.686(5)
_cell_angle_gamma                79.545(5)
_cell_formula_units_Z            2
_cell_length_a                   9.1630(5)
_cell_length_b                   11.2045(6)
_cell_length_c                   24.0190(18)
_cell_measurement_reflns_used    6018
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2650
_cell_measurement_theta_min      2.7650
_cell_volume                     2418.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'silicon plate'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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    -14.00  81.00   0.50   90.00    --    4.93  19.00  30.00  190
  2  \w    -19.00  72.00   0.50   90.00    --   -6.80  37.00 150.00  182
  3  \w    -52.00   0.00   0.50   90.00    --   -6.80 113.00 105.00  104
  4  \w    -69.00  23.00   0.50   90.00    --    4.93 -57.00-120.00  184
  5  \w    -74.00 -11.50   0.50   90.00    --   -6.80 -77.00   0.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236606000
_diffrn_orient_matrix_UB_12      -0.0540371000
_diffrn_orient_matrix_UB_13      0.0148588000
_diffrn_orient_matrix_UB_21      -0.0362516000
_diffrn_orient_matrix_UB_22      0.0278660000
_diffrn_orient_matrix_UB_23      0.0248304000
_diffrn_orient_matrix_UB_31      -0.0659097000
_diffrn_orient_matrix_UB_32      -0.0208625000
_diffrn_orient_matrix_UB_33      -0.0057320000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21954
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.17a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.912
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         8324
_refine_ls_number_restraints     851
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.1280
_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/[\s^2^(Fo^2^)+(0.1974P)^2^+66.0229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3302
_refine_ls_wR_factor_ref         0.3709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6456
_reflns_number_total             8324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00982f2.cif
_cod_data_source_block           Rutpycaphtpy
_cod_depositor_comments          'Adding full bibliography for 7707361.cif.'
_cod_original_cell_volume        2418.2(3)
_cod_database_code               7707361
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru C30 H22 N4 O4 P2 F12'
_chemical_oxdiff_usercomment     'Acetonitrile and water'
_reflns_odcompleteness_completeness 98.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.821(3)
 0.179(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{P2B, P2A}
{F6, F12A}
{F2, F11A}
{F3A, F3B}
{P1B, P1A}
{F1B, F1A}
4. Restrained distances
 F4B-F6B
 2.3 with sigma of 0.02
 F2B-F5B
 2.3 with sigma of 0.02
 F4B-F5B
 2.3 with sigma of 0.02
 F2B-F6B
 2.3 with sigma of 0.02
 F5B-F6B
 3.2 with sigma of 0.02
 F4B-F2B
 3.2 with sigma of 0.02
 P1A-F5B
 1.6 with sigma of 0.02
 P1B-F5B
 1.6 with sigma of 0.02
 P1A-F4B
 1.6 with sigma of 0.02
 P1B-F4B
 1.6 with sigma of 0.02
 F13-F18 \\sim F13-F17 \\sim F13-F14 \\sim F13-F16 \\sim F15-F18 \\sim F15-F17
\\sim F15-F14 \\sim F15-F16
 with sigma of 0.04
 P3-F13 \\sim P3-F18 \\sim P3-F15 \\sim P3-F17 \\sim P3-F14 \\sim P3-F16
 with sigma of 0.02
 F13-F15 \\sim F18-F17 \\sim F16-F14
 with sigma of 0.05
5. Uiso/Uaniso restraints and constraints
P3 \\sim F13 \\sim F18 \\sim F15 \\sim F17 \\sim F14 \\sim F16: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.2
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N7) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.2
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N3) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(P2B) = Uanis(P2A)
Uanis(F2) = Uanis(F11A)
Uiso(F6) = Uiso(F12A)
Uanis(P1B) = Uanis(P1A)
Uanis(F3A) = Uanis(F3B)
Uiso(F1B) = Uiso(F1A)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: P1A(0.6667) F4A(0.6667) F6A(0.6667) F1A(0.6667) F2A(0.6667)
 F5A(0.6667) F3A(0.6667) P2A(0.5) F7A(0.5) F12A(0.5) F11A(0.5) F8A(0.5)
 F10A(0.5) P2B(0.5) F6(0.5) F2(0.5) F9B(0.5) F10B(0.5) F7B(0.5) F8B(0.5)
 F9A(0.5) F5B(0.33333) F2B(0.33333) F6B(0.33333) F4B(0.33333) F3B(0.33333)
 P1B(0.33333) F1B(0.33333)
8.a Free rotating group:
 P3(F13,F18,F15,F17,F14,F16)
8.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C15(H15), C42(H42), C38(H38), C35(H35), C21(H21), C14(H14),
 C43(H43), C3(H3), C25(H25), C7(H7), C12(H12), C13(H13), C2(H2), C4(H4),
 C45(H45), C9(H9), C23(H23), C18(H18), C34(H34), C32(H32), C17(H17), C5(H5),
 C37(H37), C33(H33), C20(H20), C39(H39)
8.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              38085
_shelx_hkl_checksum              8367
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 5.349
_oxdiff_exptl_absorpt_empirical_full_min 0.510