Heteroleptic copper(I) complexes with coumarin-substituted aminodiphosphine and diimine ligands: synthesis and photophysical studies.
Naina, Vanitha R.; Singh, Akhil K.; Shubham, ?; Krätschmer, Frederic; Lebedkin, Sergei; Kappes, Manfred M.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02317f

data_7713817
_publ_section_title
;
 Heteroleptic copper(I) complexes with coumarin-substituted
 aminodiphosphine and diimine ligands: synthesis and photophysical
 studies.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02317f
_journal_year                    2023
_chemical_formula_moiety         'C50 H37 Cu N3 O2 P2 S, B F4, C H2 Cl2'
_chemical_formula_sum            'C51 H39 B Cl2 Cu F4 N3 O2 P2 S'
_chemical_formula_weight         1041.10
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-06-01 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.179(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8322(5)
_cell_length_b                   14.3406(3)
_cell_length_c                   17.8408(6)
_cell_measurement_reflns_used    52859
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      2.99
_cell_volume                     4550.2(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
 362 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.067
_diffrn_reflns_theta_min         2.992
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.7797
_exptl_absorpt_correction_T_min  0.2534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.447
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         11721
_refine_ls_number_restraints     633
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0680P)^2^+0.3286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8002
_reflns_number_total             11721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02317f2.cif
_cod_data_source_block           nv246a
_cod_database_code               7713817
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F3A-B1 \\sim F3B-B1
 with sigma of 0.02
 F2A-B1 \\sim F2B-B1
 with sigma of 0.02
 F4A-B1 \\sim F4B-B1
 with sigma of 0.02
 F1A-B1 \\sim F1B-B1
 with sigma of 0.02
 N3A-C47A \\sim N3B-C36B
 with sigma of 0.04
 C35A-C37A \\sim C46B-C48B
 with sigma of 0.04
 Cu-N2A \\sim Cu-N2B
 with sigma of 0.02
 Cu-N3A \\sim Cu-N3B
 with sigma of 0.02
 SA-C40A \\sim SB-C45B
 with sigma of 0.02
 SA-C41A \\sim SB-C44B
 with sigma of 0.02
 N2A-C35A \\sim N2B-C46B
 with sigma of 0.02
 N2A-C41A \\sim N2B-C44B
 with sigma of 0.02
 C41A-C43A \\sim C44B-C42B
 with sigma of 0.04
 C40A-C35A \\sim C45B-C46B
 with sigma of 0.02
 C40A-C39A \\sim C45B-C50B
 with sigma of 0.02
 C44A-C50A \\sim C41B-C39B
 with sigma of 0.04
 C45A-C49A \\sim C40B-C38B
 with sigma of 0.04
 C35A-C36A \\sim C46B-C47B
 with sigma of 0.02
 C46A-C42A \\sim C35B-C43B
 with sigma of 0.04
 C41A-C42A \\sim C44B-C43B
 with sigma of 0.02
 C35A-C41A \\sim C46B-C44B
 with sigma of 0.04
 C39A-C38A \\sim C50B-C49B
 with sigma of 0.02
 C38A-C37A \\sim C49B-C48B
 with sigma of 0.02
 C44A-C46A \\sim C41B-C35B
 with sigma of 0.04
 C36A-C37A \\sim C47B-C48B
 with sigma of 0.02
 C45A-N3A \\sim C40B-N3B
 with sigma of 0.04
 C46A-C48A \\sim C35B-C37B
 with sigma of 0.04
 C44A-C45A \\sim C41B-C40B
 with sigma of 0.02
 C44A-C43A \\sim C41B-C42B
 with sigma of 0.02
 C45A-C46A \\sim C40B-C35B
 with sigma of 0.02
 C45A-C50A \\sim C40B-C39B
 with sigma of 0.02
 C46A-N3A \\sim C35B-N3B
 with sigma of 0.02
 C46A-C47A \\sim C35B-C36B
 with sigma of 0.02
 C35A-C39A \\sim C46B-C50B
 with sigma of 0.04
 N3A-C42A \\sim N3B-C43B
 with sigma of 0.02
 C42A-C43A \\sim C43B-C42B
 with sigma of 0.02
 C41A-N3A \\sim C44B-N3B
 with sigma of 0.04
 C39A-C37A \\sim C50B-C48B
 with sigma of 0.04
 C38A-C36A \\sim C49B-C47B
 with sigma of 0.04
 C50A-C49A \\sim C39B-C38B
 with sigma of 0.02
 C49A-C48A \\sim C38B-C37B
 with sigma of 0.02
 C48A-C47A \\sim C37B-C36B
 with sigma of 0.02
 C44A-C42A \\sim C41B-C43B
 with sigma of 0.04
 C45A-C43A \\sim C40B-C42B
 with sigma of 0.04
 Cu-C35A \\sim Cu-C46B
 with sigma of 0.04
 C45A-C47A \\sim C40B-C36B
 with sigma of 0.04
 Cu-C41A \\sim Cu-C44B
 with sigma of 0.04
 Cu-C46A \\sim Cu-C35B
 with sigma of 0.04
 Cu-C42A \\sim Cu-C43B
 with sigma of 0.04
 SA-N2A \\sim SB-N2B
 with sigma of 0.04
 C46A-C50A \\sim C35B-C39B
 with sigma of 0.04
 SA-C35A \\sim SB-C46B
 with sigma of 0.04
 SA-C39A \\sim SB-C50B
 with sigma of 0.04
 SA-C42A \\sim SB-C43B
 with sigma of 0.04
 N3A-C43A \\sim N3B-C42B
 with sigma of 0.04
 N2A-C40A \\sim N2B-C45B
 with sigma of 0.04
 N2A-C36A \\sim N2B-C47B
 with sigma of 0.04
 N2A-C42A \\sim N2B-C43B
 with sigma of 0.04
 C50A-C48A \\sim C39B-C37B
 with sigma of 0.04
 C40A-C41A \\sim C45B-C44B
 with sigma of 0.04
 C49A-C47A \\sim C38B-C36B
 with sigma of 0.04
 C40A-C38A \\sim C45B-C49B
 with sigma of 0.04
 C40A-C36A \\sim C45B-C47B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
SA \\sim C50A \\sim C46A \\sim C44A \\sim N2A \\sim C42A \\sim C40A \\sim C48A
\\sim C35A \\sim C45A \\sim C41A \\sim N3A \\sim C39A \\sim C43A \\sim C38A
\\sim C49A \\sim C36A \\sim C47A \\sim C37A: within 2.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2.5A
N2B \\sim C38B \\sim C49B \\sim F3B \\sim SB \\sim C45B \\sim C41B \\sim C47B
\\sim C40B \\sim C39B \\sim C35B \\sim C44B \\sim N3B \\sim C46B \\sim C43B
\\sim C50B \\sim C42B \\sim C48B \\sim C36B \\sim C37B: within 2.5A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
4. Others
 Sof(F2B)=Sof(F4B)=Sof(F3B)=Sof(F1B)=1-FVAR(1)
 Sof(F4A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=FVAR(1)
 Sof(C41B)=Sof(H41B)=Sof(C40B)=Sof(C35B)=Sof(N3B)=Sof(C43B)=Sof(C42B)=
 Sof(H42B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=Sof(H37B)=Sof(C38B)=Sof(H38B)=
 Sof(C39B)=Sof(H39B)=Sof(SB)=Sof(C44B)=Sof(N2B)=Sof(C47B)=Sof(H47B)=Sof(C46B)=
 Sof(C45B)=Sof(C50B)=Sof(H50B)=Sof(C49B)=Sof(H49B)=Sof(C48B)=Sof(H48B)=1-FVAR(2)
 Sof(SA)=Sof(N2A)=Sof(C40A)=Sof(C35A)=Sof(C41A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=
 Sof(H38A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C44A)=Sof(H44A)=
 Sof(C45A)=Sof(C46A)=Sof(N3A)=Sof(C42A)=Sof(C43A)=Sof(H43A)=Sof(C50A)=Sof(H50A)=
 Sof(C49A)=Sof(H49A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C30(H30), C28(H28), C12(H12), C24(H24), C5(H5), C18(H18),
 C34(H34), C22(H22), C16(H16), C33(H33), C32(H32), C31(H31), C27(H27), C15(H15),
  C14(H14), C13(H13), C8(H8), C21(H21), C26(H26), C19(H19), C39A(H39A),
 C20(H20), C25(H25), C38A(H38A), C36A(H36A), C37A(H37A), C44A(H44A), C43A(H43A),
  C50A(H50A), C49A(H49A), C48A(H48A), C47A(H47A), C41B(H41B), C42B(H42B),
 C36B(H36B), C37B(H37B), C38B(H38B), C39B(H39B), C47B(H47B), C50B(H50B),
 C49B(H49B), C48B(H48B)
5.c Fitted hexagon refined as free rotating group:
 C44A(C45A,C46A,N3A,C42A,C43A), C41B(C40B,C35B,N3B,C43B,C42B), C47B(C46B,C45B,
 C50B,C49B,C48B)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              41942
_olex2_submission_special_instructions 'No special instructions were received'