Dinuclear copper(I) complexes containing pyridyl-appended diazadiphosphetidines and aminobis(diphosphonite) ligands: Synthesis, structural studies and antiproliferative activity towards human cervical, human colon carcinoma and breast cancer cells
Balakrishna, Maravanji Shivaramaiah; Rashid, Aijaz; Ananthnag, Guddekoppa S.; Naik, Susmita; Mague, Joel T.; Panda, Dulal; Dalton Transactions  (2014) –; doi:10.1039/c4dt00832d

data_7031010
_publ_section_title
;
 Dinuclear copper(I) complexes containing pyridyl-appended
 diazadiphosphetidines and aminobis(diphosphonite) ligands: Synthesis,
 structural studies and antiproliferative activity towards human cervical,
 human colon carcinoma and breast cancer cells
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/c4dt00832d
_journal_year                    2014
_chemical_formula_moiety         'C58 H57 Cu2 I2 N3 O8 P2, C2 H3 N'
_chemical_formula_sum            'C60 H60 Cu2 I2 N4 O8 P2'
_chemical_formula_weight         1407.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-04-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.464(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4841(3)
_cell_length_b                   17.0323(4)
_cell_length_c                   27.1967(7)
_cell_measurement_reflns_used    12425
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.6830
_cell_measurement_theta_min      3.2281
_cell_volume                     5765.4(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41807
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.235
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  0.6882
_exptl_absorpt_correction_T_min  0.5694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_meas      1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2828
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         10122
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+3.6021P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8320
_reflns_number_total             10122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00832d2.cif
_cod_data_source_block           msb076
_cod_database_code               7031010
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C22
 1.32 with sigma of 0.001
 C21A-C22A
 1.32 with sigma of 0.001
 C51-C52
 1.32 with sigma of 0.001
 C50-C51
 1.43 with sigma of 0.001
 C51A-C52A
 1.32 with sigma of 0.001
 C50A-C51A
 1.43 with sigma of 0.001
 C20-C22
 2.472 with sigma of 0.001
 C20-C22A
 2.472 with sigma of 0.001
 C50-C52
 2.472 with sigma of 0.001
 C50A-C52A
 2.472 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C22: 
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C21A \\sim C22A: 
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C51 \\sim C52: 
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50A \\sim C51A \\sim C52A: 
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52C)=
 Sof(H52D)=1-FVAR(1)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20(H20C,H20D), C30(H30A,H30B), C40(H40A,H40B), C50(H50A,
 H50B), C50A(H50C,H50D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C15(H15),
 C17(H17), C18(H18), C21(H21), C21A(H21A), C25(H25), C27(H27), C28(H28),
 C31(H31), C35(H35), C37(H37), C38(H38), C41(H41), C45(H45), C47(H47), C48(H48),
  C51(H51), C51A(H51A), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
5.c X=CH2 refined with riding coordinates:
 C22(H22A,H22B), C22A(H22C,H22D), C52(H52A,H52B), C52A(H52C,H52D)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C39(H39A,H39B,H39C), C49(H49A,H49B,
 H49C), C111(H11A,H11B,H11C)
;
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.569
_shelxl_version_number           2012-9