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_7713814
_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         'C46 H35 Cu N3 O3 P2, F6 P, C H2 Cl2'
_chemical_formula_sum            'C47 H37 Cl2 Cu F6 N3 O3 P3'
_chemical_formula_weight         1033.14
_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             2023-01-17
_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                 90.960(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9964(7)
_cell_length_b                   14.6953(3)
_cell_length_c                   17.3565(6)
_cell_measurement_reflns_used    36168
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      1.79
_cell_volume                     4589.5(3)
_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                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_details
;
 280 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    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28411
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.456
_diffrn_reflns_theta_min         1.789
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.7575
_exptl_absorpt_correction_T_min  0.4595
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.314
_refine_diff_density_max         1.230
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.093
_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     670
_refine_ls_number_reflns         12587
_refine_ls_number_restraints     467
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0800P)^2^+4.3553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9339
_reflns_number_total             12587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02317f2.cif
_cod_data_source_block           nv322
_cod_database_code               7713814
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.795
_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
 P3-F6A \\sim P3-F6B
 with sigma of 0.02
 P3-F4A \\sim P3-F4B
 with sigma of 0.02
 P3-F5A \\sim P3-F5B
 with sigma of 0.02
 P3-F2A \\sim P3-F2B
 with sigma of 0.02
 P3-F1A \\sim P3-F1B
 with sigma of 0.02
 P3-F3A \\sim P3-F3B
 with sigma of 0.02
 F2B-F3B \\sim F1B-F5B
 with sigma of 0.02
 F2A-F3A \\sim F1A-F5A
 with sigma of 0.02
 F6A-P3 \\sim P3-F4A
 with sigma of 0.02
 Cl1A-C47A \\sim Cl1B-C46B
 with sigma of 0.02
 Cl2A-C47A \\sim Cl2B-C46B
 with sigma of 0.02
 Cl1A-Cl2A \\sim Cl1B-Cl2B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F2B \\sim P3 \\sim F3B \\sim F1A \\sim F3A \\sim F1B \\sim F5A \\sim F4B \\sim
F5B \\sim F4A \\sim F6A \\sim F6B \\sim F2A: within 2.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2.5A
C47A \\sim Cl1A \\sim Cl2A \\sim C46B \\sim Cl2B \\sim Cl1B: within 2.5A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
4. Rigid body (RIGU) restrains
 C47A, Cl1A, Cl2A, C46B, Cl2B, Cl1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(F2B)=Sof(F1B)=Sof(F3B)=Sof(F5B)=Sof(F4B)=Sof(F6B)=1-FVAR(1)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=FVAR(1)
 Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(Cl2B)=Sof(Cl1B)=1-FVAR(2)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C47A)=Sof(H47A)=Sof(H47B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C47A(H47A,H47B), C46B(H46A,H46B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C22(H22), C28(H28), C18(H18), C24(H24), C5(H5), C30(H30),
 C34(H34), C27(H27), C21(H21), C16(H16), C6(H6), C31(H31), C19(H19), C25(H25),
 C20(H20), C46(H46), C32(H32), C26(H26), C12(H12), C35(H35), C33(H33), C45(H45),
  C14(H14), C36(H36), C38(H38), C13(H13), C15(H15), C37(H37), C44(H44), C43(H43)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              36178
_olex2_submission_special_instructions 'No special instructions were received'