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_4516137
_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_formula_moiety         'C38 H38 Cu4 I4 N8 P2'
_chemical_formula_sum            'C38 H38 Cu4 I4 N8 P2'
_chemical_formula_weight         1430.46
_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
_audit_creation_date             2016-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                69.010(2)
_cell_angle_beta                 81.979(2)
_cell_angle_gamma                71.386(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6360(2)
_cell_length_b                   10.2333(3)
_cell_length_c                   12.8232(3)
_cell_measurement_reflns_used    19561
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.2500
_cell_measurement_theta_min      2.2180
_cell_volume                     1118.36(5)
_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
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    8.00    --  -20.00   0.00-108.00  360
  2  \w    -78.00  19.00   0.50    8.00    --  -20.00 -72.00  36.00  194
  3  \w    -70.00  19.00   0.50    8.00    --  -20.00 -72.00-108.00  178
  4  \w    -39.00  -8.00   0.50    8.00    --  -20.00  72.00-180.00   62
  5  \w    -59.00 -28.50   0.50    8.00    --  -20.00  72.00-108.00   61
  6  \w    -33.50   2.50   0.50    8.00    --  -20.00 -72.00 108.00   72
  7  \w   -110.00  70.00   0.50    8.00    --  -20.00   0.00 -36.00  360
  8  \w    -72.00  19.00   0.50    8.00    --  -20.00 -72.00 -36.00  182
  9  \w    -79.00   5.00   0.50    8.00    --  -20.00 -72.00-180.00  168
 10  \w    -41.50   1.00   0.50    8.00    --  -20.00  72.00 108.00   85
 11  \w    -59.00 -28.50   0.50    8.00    --  -20.00  72.00 -36.00   61
 12  \w   -110.00  10.00   0.50    8.00    --  -20.00   0.00-180.00  240
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_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      0.0474346000
_diffrn_orient_matrix_UB_12      -0.0637541000
_diffrn_orient_matrix_UB_13      0.0363564000
_diffrn_orient_matrix_UB_21      0.0072193000
_diffrn_orient_matrix_UB_22      0.0412991000
_diffrn_orient_matrix_UB_23      0.0320201000
_diffrn_orient_matrix_UB_31      -0.0611207000
_diffrn_orient_matrix_UB_32      -0.0158720000
_diffrn_orient_matrix_UB_33      0.0341437000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21000
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.228
_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    4.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66796
_exptl_absorpt_correction_type   multi-scan
_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    2.124
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.8253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3778
_reflns_number_total             3939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02484_si_002.cif
_cod_data_source_block           compound-4
_cod_original_cell_volume        1118.35(5)
_cod_database_code               4516137
_chemical_oxdiff_formula         C17H16N3P1CuI
_reflns_odcompleteness_completeness 91.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.05
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              50533
_shelx_hkl_checksum              91489
_shelx_shelxl_version_number     2014/7
_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 4.107
_oxdiff_exptl_absorpt_empirical_full_min 0.541