Near-infrared emitting copper(i) complexes with a pyrazolylpyrimidine ligand: exploring relaxation pathways
Shekhovtsov, Nikita A.; Kokina, Tatyana E.; Vinogradova, Katerina A.; Panarin, Andrey Y.; Rakhmanova, Marianna I.; Naumov, Dmitry Y.; Pervukhina, Natalya V.; Nikolaenkova, Elena B.; Krivopalov, Viktor P.; Czerwieniec, Rafał; Bushuev, Mark B.; Dalton Transactions  (2022) –; doi:10.1039/D1DT04325K

data_7709402
_publ_section_title
;
 Near-infrared emitting copper(i) complexes with a pyrazolylpyrimidine
 ligand: exploring relaxation pathways
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04325K
_journal_year                    2022
_chemical_formula_moiety         'C42 H36 Cu N8, F6 P'
_chemical_formula_sum            'C42 H36 Cu F6 N8 P'
_chemical_formula_weight         861.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-09
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2021-07-02 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.076(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2146(2)
_cell_length_b                   18.7121(2)
_cell_length_c                   15.2367(3)
_cell_measurement_reflns_used    19318
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.9020
_cell_measurement_theta_min      3.8710
_cell_volume                     3728.46(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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     -3.00  25.00   1.00    1.50    --   36.00  95.00  71.95   28
  2  \w   -117.00 -18.00   1.00    1.50    --  -42.26 -37.00  60.00   99
  3  \w    -98.00  -2.00   1.00    1.50    --  -42.26 125.00 120.00   96
  4  \w   -100.00  -4.00   1.00    1.50    --  -42.26 128.00 -47.00   96
  5  \w   -115.00 -14.00   1.00    1.50    --  -42.26 -57.00-180.00  101
  6  \w   -117.00 -18.00   1.00    1.50    --  -42.26 -37.00 -30.00   99
  7  \w   -115.00 -14.00   1.00    1.50    --  -42.26 -57.00 -90.00  101
  8  \w     18.00  45.00   1.00    1.50    --   52.00  82.00 176.02   27
  9  \w     19.00  45.00   1.00    1.50    --   52.00  79.00 -20.54   26
 10  \w     18.00  45.00   1.00    1.50    --   52.00  81.00-100.93   27
 11  \w     18.00  45.00   1.00    1.50    --   52.00  82.00  17.58   27
 12  \w     19.00  45.00   1.00    1.50    --   52.00  79.00  60.71   26
 13  \w     19.00  45.00   1.00    1.50    --   52.00  80.00 156.75   26
 14  \w     32.00 140.00   1.00    1.50    --   64.00  76.00  65.75  108
 15  \w     35.00 144.00   1.00    1.50    --   68.00  77.00-174.07  109
 16  \w     35.00 144.00   1.00    1.50    --   68.00  77.00 124.52  109
 17  \w     36.00 144.00   1.00    1.50    --   68.00  76.00 -45.06  108
 18  \w     36.00 144.00   1.00    1.50    --   68.00  76.00 -82.69  108
 19  \w     40.00 148.00   1.00    1.50    --   72.00  76.00-110.28  108
 20  \w     97.00 148.00   1.00    1.50    --   72.00  77.00  38.13   51
 21  \w     39.00  64.00   1.00    1.50    --   72.00  77.00  -3.82   25
 22  \w    106.00 141.00   1.00    1.50    --   72.00  77.00  88.47   35
 23  \w     83.00 144.00   1.00    1.50    --   72.00  77.00-128.99   61
 24  \w     39.00  75.00   1.00    1.50    --   72.00  77.00  88.47   36
 25  \w     39.00  64.00   1.00    1.50    --   72.00  77.00-128.99   25
 26  \w     41.00  68.00   1.00    1.50    --   72.00  75.00 150.95   27
 27  \w     39.00  65.00   1.00    1.50    --   72.00  77.00  38.13   26
 28  \w     39.00 106.00   1.00    4.00    --  106.55 -94.00 -30.00   67
 29  \w     75.00 152.00   1.00    4.00    --  106.55  77.00-150.00   77
 30  \w     74.00 157.00   1.00    4.00    --  106.55  77.00 -90.00   83
 31  \w     74.00 149.00   1.00    4.00    --  106.55  77.00 -60.00   75
 32  \w     33.00 100.00   1.00    4.00    --  106.55 -94.00-180.00   67
 33  \w     80.00 139.00   1.00    4.00    --  106.55  61.00-150.00   59
 34  \w     40.00  87.00   1.00    4.00    --  106.55 -94.00  30.00   47
 35  \w    110.00 158.00   1.00    4.00    --  106.55  77.00 150.00   48
 36  \w     77.00 112.00   1.00    4.00    --  106.55  61.00  60.00   35
 37  \w     84.00 154.00   1.00    4.00    --  106.55 125.00   0.00   70
 38  \w     74.00 100.00   1.00    4.00    --  106.55  77.00   0.00   26
 39  \w     78.00 105.00   1.00    4.00    --  106.55  61.00-180.00   27
 40  \w     48.00  76.00   1.00    4.00    --  106.55 -45.00  90.00   28
 41  \w     74.00 144.00   1.00    4.00    --  106.55  77.00  60.00   70
 42  \w     42.00  77.00   1.00    4.00    --  106.55 -45.00 -60.00   35
 43  \w    106.00 151.00   1.00    4.00    --  106.55  77.00   0.00   45
 44  \w     74.00  99.00   1.00    4.00    --  106.55  77.00 150.00   25
 45  \w     74.00 149.00   1.00    4.00    --  106.55  77.00 120.00   75
 46  \w    108.00 141.00   1.00    4.00    --  106.55  77.00-180.00   33
 47  \w     44.00  73.00   1.00    4.00    --  106.55 -45.00 150.00   29
 48  \w     74.00 153.00   1.00    4.00    --  106.55  77.00 -30.00   79
 49  \w     75.00 101.00   1.00    4.00    --  106.55  77.00-180.00   26
 50  \w     35.00  66.00   1.00    4.00    --  106.55 -45.00   0.00   31
 51  \w     42.00 115.00   1.00    4.00    --  106.55-125.00 120.00   73
 52  \w     32.00 100.00   1.00    4.00    --  106.55 -94.00 120.00   68
 53  \w     74.00 151.00   1.00    4.00    --  106.55  77.00-120.00   77
 54  \w     74.00 158.00   1.00    4.00    --  106.55  77.00  90.00   84
 55  \w     24.00  75.00   1.00    4.00    --  106.55 -94.00 -60.00   51
 56  \w     77.00 104.00   1.00    4.00    --  106.55  61.00  30.00   27
 57  \w     33.00 120.00   1.00    4.00    --  106.55-125.00 -60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0307285000
_diffrn_orient_matrix_UB_12      0.0792671000
_diffrn_orient_matrix_UB_13      0.0184675000
_diffrn_orient_matrix_UB_21      -0.0716464000
_diffrn_orient_matrix_UB_22      0.0088057000
_diffrn_orient_matrix_UB_23      0.0533319000
_diffrn_orient_matrix_UB_31      0.0882335000
_diffrn_orient_matrix_UB_32      -0.0204950000
_diffrn_orient_matrix_UB_33      0.0943366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38559
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.012
_diffrn_reflns_theta_min         3.940
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0408P)^2^+4.5681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3553
_reflns_number_total             3768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04325k2.cif
_cod_data_source_block           r081
_cod_original_cell_volume        3728.43(12)
_cod_database_code               7709402
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C15(H15), C2(H2), C13(H13), C14(H14), C17(H17), C12(H12),
 C21(H21), C18(H18), C19(H19), C20(H20)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C)
;
_olex2_date_sample_data_collection 2018-10-08
_olex2_date_sample_submission    2018-10-05
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_original_sample_id KT-11
_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 3.303
_oxdiff_exptl_absorpt_empirical_full_min 0.515