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_4516135
_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         'C34 H32 Cl2 Cu2 N6 P2'
_chemical_formula_sum            'C34 H32 Cl2 Cu2 N6 P2'
_chemical_formula_weight         784.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.456(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4961(7)
_cell_length_b                   7.3977(3)
_cell_length_c                   17.2981(9)
_cell_measurement_reflns_used    12832
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3510
_cell_measurement_theta_min      2.4460
_cell_volume                     1638.22(15)
_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(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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   0.00 108.00  360
  2  \w    -24.50   7.00   0.50   12.00    --  -20.00  72.00-180.00   63
  3  \w    -25.00  70.00   0.50   12.00    --  -20.00  72.00  36.00  190
  4  \w   -110.00  56.50   0.50   12.00    --  -20.00   0.00-108.00  333
;
_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      0.0380558000
_diffrn_orient_matrix_UB_12      0.0658022000
_diffrn_orient_matrix_UB_13      -0.0003999000
_diffrn_orient_matrix_UB_21      -0.0271342000
_diffrn_orient_matrix_UB_22      0.0186122000
_diffrn_orient_matrix_UB_23      -0.0415511000
_diffrn_orient_matrix_UB_31      -0.0298287000
_diffrn_orient_matrix_UB_32      0.0671891000
_diffrn_orient_matrix_UB_33      0.0118387000
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13456
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.021
_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    1.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68078
_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    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.474
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.059
_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     208
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0360P)^2^+1.5670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2713
_reflns_number_total             2842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02484_si_002.cif
_cod_data_source_block           compound-2
_cod_database_code               4516135
_reflns_odcompleteness_completeness 91.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C1(H1), C7(H7), C3(H3A), C13(H13), C11(H11), C9(H9), C17(H17),
  C8(H8), C10(H10), C14(H14), C16(H16), C15(H15)
;
_shelx_res_checksum              37954
_shelx_hkl_checksum              54314
_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 2.262
_oxdiff_exptl_absorpt_empirical_full_min 0.688