Phosphinoamine coinage metal complexes with a coumarin fluorophore: synthesis, characterization, and <i>in vitro</i> (photo)cytotoxicity.
Naina, Vanitha R.; Shubham, ?; Rönicke, Franziska; Wagenknecht, Hans-Achim; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14701–14709; doi:10.1039/d5dt01532d

data_7719466
_publ_section_title
;
 Phosphinoamine coinage metal complexes with a coumarin fluorophore:
 synthesis, characterization, and <i>in vitro</i> (photo)cytotoxicity.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14701
_journal_page_last               14709
_journal_paper_doi               10.1039/d5dt01532d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C120 H136 Cl4 Cu4 N4 O8 P4, 10(C H2 Cl2), 0.5[CH2Cl2]'
_chemical_formula_sum            'C130.25 H156.5 Cl24.5 Cu4 N4 O8 P4'
_chemical_formula_weight         3152.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-25 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                86.002(2)
_cell_angle_beta                 78.359(2)
_cell_angle_gamma                89.766(2)
_cell_formula_units_Z            2
_cell_length_a                   15.5734(4)
_cell_length_b                   15.6178(4)
_cell_length_c                   31.5485(8)
_cell_measurement_reflns_used    105604
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      1.31
_cell_volume                     7496.8(3)
_computing_cell_refinement       'X-Area Recipe 2.0.2 (STOE, 2024)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)'
_computing_data_reduction
;
X-Area Integrate 2.5.18.0 (STOE, 2024)
X-Area LANA 2.8.4 (STOE, 2024)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            90011
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.501
_diffrn_reflns_theta_min         1.365
_diffrn_source                   'Mo Genix 3D HF'
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.7715
_exptl_absorpt_correction_T_min  0.6037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
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            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3244
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.364
_exptl_crystal_size_min          0.238
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1693
_refine_ls_number_reflns         36244
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0399P)^2^+8.0379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29474
_reflns_number_total             36244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01532d2.cif
_cod_data_source_block           nv248-3
_cod_depositor_comments
'Adding full bibliography for 7719466--7719467.cif.'
_cod_original_formula_sum        'C130.25 H156.50 Cl24.50 Cu4 N4 O8 P4'
_cod_database_code               7719466
_shelx_shelxl_version_number     2019/2
_audit_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_audit_contact_letter
;
;
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl24-C130 \\sim Cl8-C130
 with sigma of 0.02
 Cl25-C131 \\sim Cl1D-C131 \\sim Cl26-C131 \\sim Cl1E-C131
 with sigma of 0.02
 Cl23-C130 \\sim Cl1A-C130
 with sigma of 0.02
 Cl1F-C128 \\sim Cl19-C128 \\sim Cl7-C128 \\sim Cl20-C128
 with sigma of 0.02
 Cl9-C123 \\sim Cl10-C123
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1E \\sim Cl1D: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Others
 Sof(H13C)=Sof(H13D)=Sof(Cl8)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl24)=Sof(Cl23)=Sof(H13A)=Sof(H13B)=FVAR(1)
 Fixed Sof: Cl20(0.75) Cl25(0.75) Cl26(0.75) Cl19(0.75) Cl1D(0.25) Cl1E(0.25)
 Cl7(0.25) Cl1F(0.25) Cl27(0.25) Cl28(0.25) C122(0.25) H12T(0.25) H12U(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C124(H12H,H12I), C123(H12N,H12O), C125(H12F,H12G), C127(H12J,H12K), C130(H13A,
 H13B), C130(H13C,H13D), C126(H12L,H12M), C129(H12R,H12S), C121(H12P,H12Q),
 C122(H12T,H12U)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1), N4(H4), N2(H2), C96(H96), C32(H32), C2(H2A), C16(H16),
 C66(H66), C62(H62), C86(H86), C106(H106), C112(H112), C5(H5), C15(H15),
 C26(H26), C22(H22), C36(H36), C6(H6), C93(H93), C102(H102), C105(H105),
 C42(H42), C82(H82), C92(H92), C68(H68), C98(H98), C63(H63), C12(H12), C52(H52),
  C46(H46), C76(H76), C115(H115), C116(H116), C35(H35), C83(H83), C8(H8),
 C75(H75), C23(H23), C13(H13), C45(H45), C53(H53), C113(H113), C103(H103),
 C56(H56), C38(H38), C72(H72), C55(H55), C25(H25), C73(H73), C43(H43), C85(H85)
5.c Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C40(H40A,H40B,H40C), C10(H10D,H10E,H10F), C78(H78A,H78B,
 H78C), C28(H28A,H28B,H28C), C70(H70A,H70B,H70C), C59(H59A,H59B,H59C), C58(H58A,
 H58B,H58C), C120(H12A,H12B,H12C), C119(H11A,H11B,H11C), C118(H11D,H11E,H11F),
 C88(H88A,H88B,H88C), C60(H60A,H60B,H60C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C80(H80A,H80B,H80C), C79(H79A,H79B,H79C), C50(H50A,H50B,H50C), C90(H90A,
 H90B,H90C), C89(H89A,H89B,H89C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C19(H19A,H19B,H19C), C108(H10G,H10H,
 H10I), C110(H11G,H11H,H11I), C109(H10J,H10K,H10L)
;
_shelx_res_checksum              51809
_olex2_submission_special_instructions 'No special instructions were received'