Novel {Cu<sub>4</sub>} and {Cu<sub>4</sub>Cd<sub>6</sub>} clusters derived from flexible aminoalcohols: synthesis, characterization, crystal structures, and evaluation of anticancer properties.
Iman, Khushboo; Raza, Md Kausar; Ansari, Mursaleem; Monika, ?; Ansari, Azaj; Ahmad, Musheer; Ahamad, M. Naqi; Qasem, Khalil M. A.; Hussain, Sameer; Akhtar, Muhammad Nadeem; Shahid, M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11941–11953; doi:10.1039/d1dt00324k

data_7708010
_publ_section_title
;
 Novel {Cu<sub>4</sub>} and {Cu<sub>4</sub>Cd<sub>6</sub>} clusters
 derived from flexible aminoalcohols: synthesis, characterization, crystal
 structures, and evaluation of anticancer properties.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11941
_journal_page_last               11953
_journal_paper_doi               10.1039/d1dt00324k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C44 H100 Cd5.6 Cl16 Cu4.4 N8 O24, 5[CH4O], 10[H2O]'
_chemical_formula_sum            'C49 H140 Cd5.6 Cl16 Cu4.4 N8 O39'
_chemical_formula_weight         2941.90
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-22
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.02.10 svn.rb'16c95d35' for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-06-17 deposited with the CCDC.	2021-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3808(5)
_cell_length_b                   20.5924(8)
_cell_length_c                   17.6388(6)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.74
_cell_volume                     4859.0(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59705
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         2.738
_exptl_absorpt_coefficient_mu    2.664
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1578 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.9285.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       block
_exptl_crystal_F_000             2941
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         8595
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+11.7140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7253
_reflns_number_total             8595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00324k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7708010--7708011.cif.'
_cod_original_formula_sum        'C49 H140 Cd5.60 Cl16 Cu4.40 N8 O39'
_cod_database_code               7708010
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.415
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All Cl(H,H,H,H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 O10-H10
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.01
 C15-H8
 1.883886 with sigma of 0.02
 Cu2-H8
 3.036971 with sigma of 0.02
 C22-H10
 1.901004 with sigma of 0.02
 Cu2-H10
 2.659287 with sigma of 0.02
 C10-H5
 1.886691 with sigma of 0.02
 Cu1-H5
 3.041008 with sigma of 0.02
 C1-H1
 1.899223 with sigma of 0.02
 Cu1-H1
 2.682973 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl2
 with sigma of 0.04
 C13-C14 \\sim C13-C14A
 with sigma of 0.02
 O9-C14 \\sim O9A-C14A
 with sigma of 0.02
 O9-C13 \\sim O9A-C13
 with sigma of 0.04
 O12-C21 \\sim O12A-C21A
 with sigma of 0.02
 C19-C21 \\sim C19-C21A
 with sigma of 0.02
 O12-C19 \\sim O12A-C19
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cu3 \\sim Cd1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 Cl2, Cd1, Cl1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cu3, Cl8, Cl1A, Cl2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O9, H3A, C13, C14, O9A, C14A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O12A)=Sof(H12C)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(1)
 Sof(O12)=Sof(H12)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(1)
 Fixed Sof: Cd1(0.8) Cl1(0.8) O9(0.5) H9(0.5) C14(0.5) H14A(0.5) H14B(0.5)
 Cl8B(0.8) Cl8(0.2) Cl1A(0.2) O9A(0.5) H9AA(0.5) C14A(0.5) H14C(0.5) H14D(0.5)
 Cu3(0.2)
 Fixed Uiso: O12A(0.03) C21A(0.03)
6.a Ternary CH refined with riding coordinates:
 N1(H1A), N2(H2A), N3(H3A), N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1(H1B,H1C), C3(H3B,H3C), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,
 H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
  C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C14A(H14C,H14D), C21A(H21C,H21D)
6.c Tetrahedral OH refined with riding coordinates:
 O2(H2)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O9(H9), O11(H11), O12(H12), O9A(H9AA), O12A(H12C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 377 electrons were 
found in a volume of 1025\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 5[CH4O], 10[H2O] per Formula Unit 
which account for 380 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94361
_shelx_hkl_checksum              19320
_shelx_fab_checksum              35148
_olex2_submission_special_instructions 'No special instructions were received'