Syntheses, crystal structures, magnetic properties and ESI-MS studies of a series of trinuclear CuIIMIICuII compounds (M = Cu, Ni, Co, Fe, Mn, Zn)
Hari, Nairita; Mandal, Shuvankar; Jana, Arpita; Sparkes, Hazel A.; Mohanta, Sasankasekhar; RSC Advances 8 (2018) 7315–; doi:10.1039/C7RA13763J

data_7230171
_publ_section_title
;
 Syntheses, crystal structures, magnetic properties and ESI-MS studies of
 a series of trinuclear CuIIMIICuII compounds (M = Cu, Ni, Co, Fe, Mn, Zn)
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              7315
_journal_paper_doi               10.1039/C7RA13763J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C42 H48 Cu2 N4 O6 Zn, 2(Cl O4)'
_chemical_formula_sum            'C42 H48 Cl2 Cu2 N4 O14 Zn'
_chemical_formula_weight         1096.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-01 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.149(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.200(19)
_cell_length_b                   12.254(15)
_cell_length_c                   24.32(3)
_cell_measurement_reflns_used    2567
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.761
_cell_measurement_theta_min      2.453
_cell_volume                     4588(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker Apex suite'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1132
_diffrn_reflns_av_unetI/netI     0.1302
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13690
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.124
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.1831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.476
_refine_diff_density_min         -2.040
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4018
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0943
_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^)+(0.1742P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2452
_reflns_number_total             4018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra13763j2.cif
_cod_data_source_block           6
_cod_original_cell_volume        4589(9)
_cod_database_code               7230171
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.357
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3A
 0.85 with sigma of 0.01
 C21-H3A
 1.886791 with sigma of 0.02
 Zn1-H3A
 2.667193 with sigma of 0.02
 Cl1-O4 \\sim Cl1-O7 \\sim Cl1-O5B \\sim Cl1-O5A \\sim Cl1-O6B \\sim Cl1-O6A
 with sigma of 0.01
 C13-C12 \\sim C13A-C12A \\sim C12A-C11A \\sim C12-C11 \\sim C11-C10 \\sim
C11A-C10A \\sim C9A-C10A ~
 C9-C10 \\sim C9A-C8A \\sim C9-C8 \\sim C8-C13 \\sim C8A-C13A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim O4 \\sim O6A \\sim O7 \\sim O5A \\sim O5B \\sim O6B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C13A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O6B) = Uanis(O6A)
Uanis(O5B) = Uanis(O5A)
Uanis(C12A) = Uanis(C12)
4. Others
 Sof(C13A)=Sof(H13A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=
 Sof(H12D)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13)=
 FVAR(1)
 Sof(O5B)=Sof(O6B)=1-FVAR(2)
 Sof(O6A)=Sof(O5A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C13A(H13A), C8A(H8A)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C9A(H9AA,H9AB),
 C10A(H10C,H10D), C11A(H11C,H11D), C12A(H12C,H12D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              39868
_olex2_submission_special_instructions 'No special instructions were received'