Diverse Architectures and Luminescence Properties of Group 11 Complexes Containing Pyrimidine-Based Phosphine, <i>N</i>-((Diphenylphosphine)methyl)pyrimidin-2-amine.
Kumar, Saurabh; Mondal, Dipanjan; Balakrishna, Maravanji S.; ACS omega 3 (2018) 16601–16614; doi:10.1021/acsomega.8b02484

data_4516138
_publ_section_title
;
 Diverse Architectures and Luminescence Properties of Group 11 Complexes
 Containing Pyrimidine-Based Phosphine,
 <i>N</i>-((Diphenylphosphine)methyl)pyrimidin-2-amine.
;
_journal_issue                   12
_journal_name_full               'ACS omega'
_journal_page_first              16601
_journal_page_last               16614
_journal_paper_doi               10.1021/acsomega.8b02484
_journal_volume                  3
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H32 Ag2 F6 N6 O6 P2 S2'
_chemical_formula_sum            'C36 H32 Ag2 F6 N6 O6 P2 S2'
_chemical_formula_weight         1100.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3162(3)
_cell_length_b                   18.1124(7)
_cell_length_c                   23.9326(9)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0530
_cell_measurement_theta_min      2.3190
_cell_volume                     4038.4(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -110.00  70.00   0.50   12.00    --  -20.00   0.00-180.00  360
  2  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00  36.00  258
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0747116000
_diffrn_orient_matrix_UB_12      -0.0010288000
_diffrn_orient_matrix_UB_13      -0.0055960000
_diffrn_orient_matrix_UB_21      0.0017404000
_diffrn_orient_matrix_UB_22      -0.0379286000
_diffrn_orient_matrix_UB_23      0.0073567000
_diffrn_orient_matrix_UB_31      -0.0144221000
_diffrn_orient_matrix_UB_32      -0.0097438000
_diffrn_orient_matrix_UB_33      -0.0281602000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22618
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.249
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88356
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.810
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7072
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0240P)^2^+10.0840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6566
_reflns_number_total             7072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02484_si_002.cif
_cod_data_source_block           compound-5
_cod_database_code               4516138
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H16 N3 P F3 S O3 Ag'
_reflns_odcompleteness_completeness 90.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.07
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(4) 0.51(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(F3B) \\sim Ueq, Uanis(C35B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F1B)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(C35A) \\sim Ueq,
Uanis(F3A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Sof(F3B)=Sof(C35B)=Sof(F2B)=Sof(F1B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(C35A)=Sof(F3A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C24(H24), C18(H18), N6(H6), C20(H20), C2(H2), C26(H26), C14(H14),
 N3(H3), C25(H25), C9(H9), C10(H10), C33(H33), C16(H16), C3(H3A), C31(H31),
 C34(H34), C27(H27), C28(H28), C8(H8), C7(H7), C1(H1), C13(H13), C30(H30),
 C17(H17), C15(H15), C32(H32), C11(H11)
;
_shelx_res_checksum              14994
_shelx_hkl_checksum              47907
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.961
_oxdiff_exptl_absorpt_empirical_full_min 0.587