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_7713813
_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 H36 Cu N4 O2 P2, F6 P, C4 H10 O'
_chemical_formula_sum            'C50 H46 Cu F6 N4 O3 P3'
_chemical_formula_weight         1021.36
_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'
_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                 92.318(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8014(8)
_cell_length_b                   14.6604(6)
_cell_length_c                   17.7919(7)
_cell_measurement_reflns_used    23836
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.29
_cell_measurement_theta_min      1.80
_cell_volume                     4639.5(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    'olex2.solve 1.5-alpha (Bourhis et al., 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 0.990
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_details
;
 290 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  0.0395
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30397
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.280
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.7831
_exptl_absorpt_correction_T_min  0.5082
_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    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.382
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         12721
_refine_ls_number_restraints     740
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0996P)^2^+1.9814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8214
_reflns_number_total             12721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02317f2.cif
_cod_data_source_block           nv321
_cod_database_code               7713813
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P3-F1 \\sim P3-F1A
 with sigma of 0.02
 P3-F5 \\sim P3-F5A
 with sigma of 0.02
 P3-F2 \\sim P3-F2A
 with sigma of 0.02
 P3-F4 \\sim P3-F4A
 with sigma of 0.02
 P3-F6 \\sim P3-F6A
 with sigma of 0.02
 P3-F3 \\sim P3-F3A
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C50 \\sim O3 \\sim C49 \\sim C48 \\sim C47: within 2.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2.5A
P3 \\sim F3 \\sim F3A \\sim F2A \\sim F2 \\sim F4 \\sim F4A \\sim F6A \\sim F6
\\sim F5A \\sim F5 \\sim F1 \\sim F1A: within 2.5A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2.5A
Uanis(C50) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(P3) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F6A) \\sim
Ueq, Uanis(F5A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F2A) \\sim Ueq,
Uanis(F1A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C50) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Others
 Sof(F3A)=Sof(F2A)=Sof(F4A)=Sof(F6A)=Sof(F5A)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F5)=Sof(F2)=Sof(F4)=Sof(F6)=Sof(F3)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C48(H48A,H48B)
6.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C16(H16), C2(H2), C6(H6), C3(H3), C15(H15), C22(H22), C14(H14),
 C18(H18), C34(H34), C24(H24), C12(H12), C30(H30), C35(H35), C45(H45), C31(H31),
  C13(H13), C8(H8), C25(H25), C32(H32), C33(H33), C28(H28), C38(H38), C36(H36),
 C26(H26), C44(H44), C37(H37), C42(H42), C43(H43), C21(H21), C20(H20), C27(H27),
  C19(H19)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C50(H50A,H50B,H50C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              54633
_olex2_submission_special_instructions 'No special instructions were received'