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_7046678
_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         'C44 H62 Cu3 N10 O5, C H4 O'
_chemical_formula_sum            'C45 H66 Cu3 N10 O6'
_chemical_formula_weight         1033.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                69.458(2)
_cell_angle_beta                 80.002(3)
_cell_angle_gamma                80.362(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1014(8)
_cell_length_b                   15.2651(10)
_cell_length_c                   15.6289(10)
_cell_measurement_reflns_used    32249
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.109
_cell_measurement_theta_min      2.364
_cell_volume                     2644.7(3)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32249
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.109
_diffrn_reflns_theta_max         25.109
_diffrn_reflns_theta_min         2.364
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9275
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0218P)^2^+5.6240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7682
_reflns_number_total             9275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01400k2.cif
_cod_data_source_block           2
_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_database_code               7046678
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.865
_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, All O(H,H) groups
2. Restrained distances
 N2-C13 \\sim N2-C13A
 with sigma of 0.02
 N2-C11 \\sim N2-C11A
 with sigma of 0.04
 N2-C12 \\sim N2-C12A
 with sigma of 0.04
 C10-C11 \\sim C10-C11A
 with sigma of 0.04
 C10-C12 \\sim C10-C12A
 with sigma of 0.04
 C11-C12 \\sim C11A-C12A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C10, C11A, N2, C13A, C12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C13A)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: H32A(0.5) H32B(0.5) H32C(0.5) H32D(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1AA(0.5) H1AD(0.5) H1AE(0.5)
 C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) H1CC(0.5)
 C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
5.a Rotating group:
 O5(H5A,H5B)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C14(H14A,H14B), C9(H9A,H9B), C32(H32A,H32B), C32(H32C,H32D),
 C10(H10A,H10B), C10(H10C,H10D), C36(H36A,H36B), C11(H11A,H11B), C0AA(H0AA,
 H0AB), C1AA(H1AD,H1AE), C11A(H11C,H11D)
5.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C27(H27), C42(H42), C18(H18), C25(H25), C5(H5), C3(H3), C40(H40)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C7(H7A,H7B,H7C), C13(H13A,H13B,
 H13C), C44(H44A,H44B,H44C), C29(H29A,H29B,H29C), C8(H8A,H8B,H8C), C21(H21A,
 H21B,H21C), C46(H46A,H46B,H46C), C12(H12A,H12B,H12C), C43(H43A,H43B,H43C),
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,
 H1DC), C13A(H13D,H13E,H13F), C12A(H12D,H12E,H12F)
5.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              16375
_shelx_fab_checksum              67594
_olex2_submission_special_instructions 'No special instructions were received'