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_7230170
_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 Mn N4 O6, 2(Cl O4)'
_chemical_formula_sum            'C42 H48 Cl2 Cu2 Mn N4 O14'
_chemical_formula_weight         1085.76
_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             2018-01-29
_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                 108.528(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.287(9)
_cell_length_b                   12.113(6)
_cell_length_c                   24.283(13)
_cell_measurement_reflns_used    4334
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.148
_cell_measurement_theta_min      2.468
_cell_volume                     4542(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16140
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.550
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0745 before and 0.0447 after correction. The Ratio of minimum to maximum transmission is 0.8536. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4230
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0504P)^2^+4.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3354
_reflns_number_total             4230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra13763j2.cif
_cod_data_source_block           5
_cod_database_code               7230170
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.851
_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. Shared sites
{C12B, C12A}
3. Restrained distances
 O3-H3A
 0.85 with sigma of 0.01
 C21-H3A
 1.883486 with sigma of 0.02
 Mn1-H3A
 2.735138 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
 C9B-C8B \\sim C9A-C8A \\sim C9B-C10B \\sim C9A-C10A \\sim C11B-C10B \\sim
C11A-C10A \\sim C12B-C11B ~
 C12A-C11A \\sim C13A-C12A \\sim C13B-C12B \\sim C8B-C13B \\sim C8A-C13A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim O4 \\sim O6A \\sim O7 \\sim O5A \\sim O6B \\sim O5B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C9A \\sim C11A \\sim C12A \\sim C13A \\sim C10A \\sim C10B \\sim C9B \\sim C11B
\\sim C13B \\sim C12B \\sim C8A \\sim C8B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O6B) = Uanis(O6A)
Uanis(C12A) = Uanis(C12B)
Uanis(C11B) = Uanis(C11A)
Uanis(C12B) = Uanis(C12A)
5. Others
 Sof(C8B)=Sof(H8B)=Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C13B)=Sof(H13B)=Sof(C12B)=Sof(H12C)=
 Sof(H12D)=1-FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=
 Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=Sof(C8A)=Sof(H8A)=Sof(C10A)=Sof(H10A)=
 Sof(H10B)=FVAR(1)
 Sof(O6B)=Sof(O5B)=1-FVAR(2)
 Sof(O6A)=Sof(O5A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C13A(H13A), C8A(H8A), C8B(H8B), C13B(H13B)
6.b Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), C11A(H11A,H11B), C12A(H12A,H12B), C10A(H10A,H10B), C10B(H10C,
 H10D), C9B(H9BA,H9BB), C11B(H11C,H11D), C12B(H12C,H12D)
6.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)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              1734
_olex2_submission_special_instructions 'No special instructions were received'