Ag(i) complex design affording intense phosphorescence with a landmark lifetime of over 100 milliseconds.
Shafikov, Marsel Z.; Czerwieniec, Rafał; Yersin, Hartmut; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2802–2806; doi:10.1039/c8dt04078h

data_7048390
_publ_section_title
;
 Ag(i) complex design affording intense phosphorescence with a landmark
 lifetime of over 100 milliseconds.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2802
_journal_page_last               2806
_journal_paper_doi               10.1039/c8dt04078h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C50 H40 Ag N2 O P2, C0.6 H1.2 Cl0.9, 0.3(Cl), F6 P, 0.4(C H2 Cl2)'
_chemical_formula_sum            'C51 H42 Ag Cl2 F6 N2 O P3'
_chemical_formula_weight         1084.54
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-07
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-10-11 deposited with the CCDC.
2018-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                106.306(3)
_cell_angle_beta                 98.251(3)
_cell_angle_gamma                103.499(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0617(4)
_cell_length_b                   12.1065(4)
_cell_length_c                   19.4649(8)
_cell_measurement_reflns_used    8006
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.4610
_cell_measurement_theta_min      3.8760
_cell_volume                     2370.92(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41h (Rigaku OD, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.953
_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    -75.00  38.00   1.00    1.00    --  -40.89  77.00-120.00  113
  2  \w    -75.00  38.00   1.00    1.00    --  -40.89  77.00 120.00  113
  3  \w    -70.00  33.00   1.00    1.00    --  -40.89  57.00  30.00  103
  4  \w     77.00 158.00   1.00    3.00    --  106.98  61.00 150.00   81
  5  \w     29.00  69.00   1.00    3.00    --  106.98 -30.00  30.00   40
  6  \w     32.00  77.00   1.00    3.00    --  106.98 -45.00 -90.00   45
  7  \w     32.00 121.00   1.00    3.00    --  106.98-125.00-120.00   89
  8  \w     23.00 109.00   1.00    3.00    --  106.98 -94.00 -60.00   86
  9  \w     46.00 158.00   1.00    3.00    --  106.98  15.00 -30.00  112
 10  \w     29.00  69.00   1.00    3.00    --  106.98 -30.00   0.00   40
 11  \w     29.00  69.00   1.00    3.00    --  106.98 -30.00 150.00   40
 12  \w     32.00 121.00   1.00    3.00    --  106.98-125.00-180.00   89
 13  \w     32.00  77.00   1.00    3.00    --  106.98 -45.00 120.00   45
 14  \w     29.00  69.00   1.00    3.00    --  106.98 -30.00 -30.00   40
 15  \w     28.00 141.00   1.00    3.00    --  106.98 -77.00   0.00  113
 16  \w     73.00 158.00   1.00    3.00    --  106.98 125.00   0.00   85
 17  \w   -115.00 -75.00   1.00    1.00    --  -40.89 -57.00  30.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1017143000
_diffrn_orient_matrix_UB_12      0.0576839000
_diffrn_orient_matrix_UB_13      -0.0358642000
_diffrn_orient_matrix_UB_21      0.0800673000
_diffrn_orient_matrix_UB_22      0.0825377000
_diffrn_orient_matrix_UB_23      0.0765088000
_diffrn_orient_matrix_UB_31      0.0695770000
_diffrn_orient_matrix_UB_32      -0.0950304000
_diffrn_orient_matrix_UB_33      0.0044203000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18013
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.667
_diffrn_reflns_theta_min         3.922
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41h (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         9130
_refine_ls_number_restraints     457
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0502P)^2^+0.5492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7994
_reflns_number_total             9130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04078h2.cif
_cod_data_source_block           p003
_cod_depositor_comments          'Adding full bibliography for 7048390.cif.'
_cod_original_cell_volume        2370.92(16)
_cod_database_code               7048390
_chemical_oxdiff_formula         'C50 H40 N2 P3 O F6 Ag'
_chemical_oxdiff_usercomment     'Shafikoy MZR-02'
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 Cl1_4-C1_4 \\sim Cl2_4-C1_4
 with sigma of 0.01
 P1_1-F1_1 \\sim P1_1-F2_1 \\sim P1_1-F3_1 \\sim P1_1-F4_1 \\sim P1_1-F5_1
\\sim P1_1-F6_1
 P1_2-F1_2 \\sim P1_2-F2_2 \\sim P1_2-F3_2 \\sim P1_2-F4_2 \\sim P1_2-F5_2
\\sim P1_2-F6_2
 with sigma of 0.02
 F1_1-F2_1 \\sim F1_1-F4_1 \\sim F1_1-F5_1 \\sim F1_1-F6_1 \\sim F3_1-F2_1
\\sim F3_1-F4_1 \\sim F3_1-
 F5_1 \\sim F3_1-F6_1 \\sim F4_1-F1_1 \\sim F4_1-F3_1 \\sim F2_1-F3_1 \\sim
F2_1-F1_1
 F1_2-F2_2 \\sim F1_2-F4_2 \\sim F1_2-F5_2 \\sim F1_2-F6_2 \\sim F3_2-F2_2
\\sim F3_2-F4_2 \\sim F3_2-
 F5_2 \\sim F3_2-F6_2 \\sim F4_2-F1_2 \\sim F4_2-F3_2 \\sim F2_2-F3_2 \\sim
F2_2-F1_2
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P1_1 \\sim F1_1 \\sim F2_1 \\sim F3_1 \\sim F4_1 \\sim F5_1 \\sim F6_1 \\sim
P1_2 \\sim F1_2 \\sim F2_2 \\sim F3_2 \\sim F4_2 \\sim F5_2 \\sim F6_2: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Cl1_4 \\sim Cl2_4 \\sim C1_4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
F4_2 \\sim Cl2 \\sim Cl2X: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
P1_2 \\sim F1_2 \\sim F2_2 \\sim F3_2 \\sim F4_2 \\sim F5_2 \\sim F6_2 \\sim
C0AA \\sim Cl1 \\sim Cl2: within 2.5A with sigma of 0.01 and sigma for terminal
atoms of 0.01
4. Others
 Fixed Sof: Cl1(0.6) Cl2(0.3) C0AA(0.6) H0Aa(0.6) H0Ab(0.6) Cl2X(0.3) P1(0.6)
 F1(0.6) F2(0.6) F3(0.6) F4(0.6) F5(0.6) F6(0.6) P1(0.4) F1(0.4) F2(0.4)
 F3(0.4) F4(0.4) F5(0.4) F6(0.4) Cl1(0.4) Cl2(0.4) C1(0.4) H1a(0.4) H1b(0.4)
5.a Everything fixed:
 H0Aa, H0Ab
5.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b)
5.c Aromatic/amide H refined with riding coordinates:
 C46(H46), C16(H16), C22(H22), C41(H41), C47(H47), C26(H26), C20(H20),
 C25(H25), C48(H48), C49(H49), C23(H23), C17(H17), C29(H29), C42(H42), C44(H44),
  C28(H28), C34(H34), C30(H30), C43(H43), C24(H24), C32(H32), C18(H18),
 C31(H31), C19(H19), C35(H35), C3(H3), C38(H38), C11(H11), C8(H8), C4(H4),
 C7(H7), C37(H37), C12(H12), C36(H36)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C14(H14a,H14b,H14c)
;
_shelx_res_checksum              27034
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-07
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_original_sample_id MZR-02
_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 1.571
_oxdiff_exptl_absorpt_empirical_full_min 0.571