Non-conventional synthesis and photophysical studies of platinum(ii) complexes with methylene bridged 2,2'-dipyridylamine derivatives.
Bulatov, Evgeny; Haukka, Matti; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3369–3379; doi:10.1039/c8dt03912g

data_7049088
_publ_section_title
;
 Non-conventional synthesis and photophysical studies of platinum(ii)
 complexes with methylene bridged 2,2'-dipyridylamine derivatives.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3369
_journal_page_last               3379
_journal_paper_doi               10.1039/c8dt03912g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C24 H20 N5 O4, Br'
_chemical_formula_sum            'C24 H20 Br N5 O4'
_chemical_formula_weight         522.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-09-21 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5826(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.23630(4)
_cell_length_b                   14.82926(10)
_cell_length_c                   18.24598(11)
_cell_measurement_reflns_used    21103
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.6810
_cell_measurement_theta_min      3.8190
_cell_volume                     2227.68(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -113.00  -22.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -77.0000 -150.0000 91

  2 omega  -41.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   37.0000 -180.0000 73

  3 omega -104.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -77.0000  120.0000 91

  4 omega -113.00  -26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -37.0000    0.0000 87

  5 omega -100.00  -65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176 -152.0000 -146.0000 35

  6 omega   67.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176   37.0000  -30.0000 25

  7 omega  124.00  159.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  120.0000 35

  8 omega   82.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000    0.0000 26

  9 omega   92.00  138.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -90.0000 46

 10 omega   74.00   99.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 25

 11 omega   68.00  116.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  150.0000 48

 12 omega   70.00   95.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 25

 13 omega   74.00   99.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 25

 14 omega   35.00   61.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -90.0000 26

 15 omega   46.00   72.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 26

 16 omega   33.00   59.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000    0.0000 26

 17 omega   54.00   80.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   30.0000 26

 18 omega  101.00  142.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -150.0000 41

 19 omega  113.00  142.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   30.0000 29

 20 omega   83.00  112.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -120.0000 29

 21 omega   88.00  114.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 26

 22 omega   59.00   91.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 32

 23 omega  117.00  148.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -150.0000 31

 24 omega   43.00   76.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 33

 25 omega   68.00  114.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 46

 26 omega   98.00  142.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   60.0000 44

 27 omega  152.00  177.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   96.0000 -158.0000 25

 28 omega   39.00   98.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 59

 29 omega   93.00  119.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000    0.0000 26

 30 omega  143.00  175.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000    0.0000 32

 31 omega  109.00  145.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000   90.0000 36

 32 omega   36.00   70.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 34

 33 omega  134.00  159.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -60.0000 25

 34 omega   30.00   67.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  120.0000 37

 35 omega   83.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 25

 36 omega   70.00  115.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 45

 37 omega   60.00   95.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  150.0000 35

 38 omega  101.00  148.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -120.0000 47

 39 omega  112.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 66

 40 omega  134.00  176.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  150.0000 42

 41 omega   79.00  105.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -120.0000 26

 42 omega  110.00  135.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -120.0000 25

 43 omega   38.00   90.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 52

 44 omega   60.00  102.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000 -150.0000 42

 45 omega  130.00  156.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000 -150.0000 26

 46 omega   69.00   94.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -150.0000 25

 47 omega   72.00  100.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -90.0000 28

 48 omega  100.00  138.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000  -60.0000 38

 49 omega   87.00  113.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 26

 50 omega  147.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 31

 51 omega   66.00  100.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -150.0000 34

 52 omega   90.00  139.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -120.0000 49

 53 omega   67.00   94.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000   30.0000 27

 54 omega   49.00   84.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   90.0000 35

 55 omega   35.00   99.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000   90.0000 64

 56 omega   49.00   85.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 36

 57 omega   73.00   98.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   30.0000 25

 58 omega   60.00   86.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000   60.0000 26

 59 omega   89.00  145.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -60.0000 56

 60 omega  116.00  141.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000    0.0000 25

 61 omega   88.00  137.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  150.0000 49

 62 omega   69.00  103.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -69.0000  164.8669 34
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0431465000
_diffrn_orient_matrix_UB_12      -0.0814402000
_diffrn_orient_matrix_UB_13      -0.0492039000
_diffrn_orient_matrix_UB_21      0.0515944000
_diffrn_orient_matrix_UB_22      0.0535795000
_diffrn_orient_matrix_UB_23      -0.0678439000
_diffrn_orient_matrix_UB_31      0.1745995000
_diffrn_orient_matrix_UB_32      -0.0359531000
_diffrn_orient_matrix_UB_33      0.0104596000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31951
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.749
_diffrn_reflns_theta_min         3.842
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.882
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.1338
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.0594
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0316P)^2^+1.3457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4575
_reflns_number_total             4685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03912g2.cif
_cod_data_source_block           eb104_m
_cod_depositor_comments
'Adding full bibliography for 7049077--7049089.cif.'
_cod_database_code               7049088
_chemical_oxdiff_formula         'C24 H24 N5 O4'
_chemical_oxdiff_usercomment     'Clear, light brown, block 0.15 0.15 0.15'
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.699
_reflns_odcompleteness_completeness 98.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              93269
_shelx_shelxl_version_number     2014/7
_ins_header
;
TITL EB104_m in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   8.236302  14.829261  18.245975  90.0000  91.5826  90.0000
ZERR    4.00   0.000044   0.000095   0.000114   0.0000   0.0005   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O
UNIT 96.00 96.00 20.00 16.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'