Mixed azido/phenoxido bridged trinuclear Cu(ii) complexes of Mannich bases: Synthesis, structures, magnetic properties and catalytic oxidase activities.
Das, Avijit; Bhattacharya, Kisholoy; Das, Lakshmi Kanta; Giri, Sanjib; Ghosh, Ashutosh; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9385–9399; doi:10.1039/c8dt01400k

data_7046679
_publ_section_title
;
 Mixed azido/phenoxido bridged trinuclear Cu(ii) complexes of Mannich
 bases: Synthesis, structures, magnetic properties and catalytic oxidase
 activities.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9385
_journal_page_last               9399
_journal_paper_doi               10.1039/c8dt01400k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C48 H68 Cu3 N10 O4, 2(C H4 O), H2 O'
_chemical_formula_sum            'C50 H78 Cu3 N10 O7'
_chemical_formula_weight         1121.84
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-28 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.238(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.606(3)
_cell_length_b                   19.878(4)
_cell_length_c                   19.445(4)
_cell_measurement_reflns_used    39801
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.219
_cell_measurement_theta_min      1.395
_cell_volume                     5641(2)
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_collection       'BRUKER APEX-II'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_measurement_method       OMEGA-SCAN
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39801
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.219
_diffrn_reflns_theta_max         25.219
_diffrn_reflns_theta_min         1.395
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         10061
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0635P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6429
_reflns_number_total             10061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01400k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7046677--7046679.cif.
;
_cod_original_cell_volume        5641.3(19)
_cod_database_code               7046679
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.872
_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, All O(H) groups
2. Restrained distances
 O5-H5A
 0.96 with sigma of 0.02
 O5-H5B
 0.96 with sigma of 0.02
 O6-H6
 0.9 with sigma of 0.02
 Cu3-N4 \\sim Cu3-N4A
 with sigma of 0.02
 N4-C37 \\sim N4A-C37A
 with sigma of 0.02
 N4-C35 \\sim N4A-C35A
 with sigma of 0.02
 N4-C34 \\sim N4A-C34A
 with sigma of 0.02
 C33-C34 \\sim C33-C34A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 Cu3-C37 \\sim Cu3-C37A
 with sigma of 0.04
 Cu3-C35 \\sim Cu3-C35A
 with sigma of 0.04
 Cu3-C34 \\sim Cu3-C34A
 with sigma of 0.04
 N4-C33 \\sim N4A-C33
 with sigma of 0.04
 N4-C36 \\sim N4A-C36A
 with sigma of 0.04
 N4-C38 \\sim N4A-C38A
 with sigma of 0.04
 C37-C35 \\sim C37A-C35A
 with sigma of 0.04
 C37-C34 \\sim C37A-C34A
 with sigma of 0.04
 C35-C34 \\sim C35A-C34A
 with sigma of 0.04
 Cu1-N2 \\sim Cu1-N2A
 with sigma of 0.02
 N2-C14 \\sim N2A-C14A
 with sigma of 0.02
 N2-C12 \\sim N2A-C12A
 with sigma of 0.02
 N2-C11 \\sim N2A-C11A
 with sigma of 0.02
 C10-C11 \\sim C10-C11A
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 Cu1-C14 \\sim Cu1-C14A
 with sigma of 0.04
 Cu1-C12 \\sim Cu1-C12A
 with sigma of 0.04
 Cu1-C11 \\sim Cu1-C11A
 with sigma of 0.04
 N2-C10 \\sim N2A-C10
 with sigma of 0.04
 N2-C15 \\sim N2A-C15A
 with sigma of 0.04
 N2-C13 \\sim N2A-C13A
 with sigma of 0.04
 C14-C12 \\sim C14A-C12A
 with sigma of 0.04
 C14-C11 \\sim C14A-C11A
 with sigma of 0.04
 C12-C11 \\sim C12A-C11A
 with sigma of 0.04
3. Rigid bond restraints
 C34, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C36: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of
0.009 and sigma for terminal atoms of 0.018
5. Rigid body (RIGU) restrains
 N4A, C37A, C35A, C34A, C36A, C38A, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, N2A, C14A, C12A, C15A, C11A, C13A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H33C)=Sof(H33D)=Sof(N4A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(N4)=Sof(H33A)=Sof(H33B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(H10C)=Sof(H10D)=Sof(N2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C12A)=
 Sof(H12C)=Sof(H12D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C11A)=
 Sof(H11C)=Sof(H11D)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(2)
 Sof(N2)=Sof(H10A)=Sof(H10B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C32(H32A,H32B), C9(H9A,H9B), C10(H10A,H10B), C10(H10C,H10D),
 C33(H33A,H33B), C33(H33C,H33D), C39(H39A,H39B), C14(H14A,H14B), C12(H12A,H12B),
  C37(H37A,H37B), C11(H11A,H11B), C35(H35A,H35B), C34(H34A,H34B), C37A(H37C,
 H37D), C35A(H35C,H35D), C34A(H34C,H34D), C14A(H14C,H14D), C12A(H12C,H12D),
 C11A(H11C,H11D)
7.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C5(H5), C43(H43), C20(H20), C3(H3), C28(H28), C26(H26), C41(H41)
7.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C22(H22A,H22B,H22C), C7(H7A,H7B,
 H7C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C), C49(H49A,
 H49B,H49C), C30(H30A,H30B,H30C), C8(H8A,H8B,H8C), C46(H46A,H46B,H46C),
 C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C38(H38A,H38B,H38C), C36A(H36D,H36E,
 H36F), C38A(H38D,H38E,H38F), C15A(H15D,H15E,H15F), C13A(H13D,H13E,H13F)
7.d Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              21290
_olex2_submission_special_instructions 'No special instructions were received'