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_7230169
_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 Fe N4 O6, 2(Cl O4)'
_chemical_formula_sum            'C42 H48 Cl2 Cu2 Fe N4 O14'
_chemical_formula_weight         1086.67
_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                 107.775(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0994(12)
_cell_length_b                   12.1164(9)
_cell_length_c                   24.2086(18)
_cell_measurement_reflns_used    9555
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.642
_cell_measurement_theta_min      2.467
_cell_volume                     4496.9(6)
_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 0.998
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24823
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.694
_diffrn_reflns_theta_min         1.767
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0830 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.7637. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0487P)^2^+16.1235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3617
_reflns_number_total             4256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra13763j2.cif
_cod_data_source_block           4
_cod_database_code               7230169
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.823
_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
 O3-H3A
 0.85 with sigma of 0.01
 C21-H3A
 1.889664 with sigma of 0.02
 Fe1-H3A
 2.66108 with sigma of 0.02
 C13-C12 \\sim C9-C10 \\sim C12-C11 \\sim C10-C11
 with sigma of 0.01
 C13-C8A \\sim C13-C8B \\sim C9-C8A \\sim C9-C8B
 with sigma of 0.01
 Cl1-O6A \\sim Cl1-O6B \\sim Cl1-O5A \\sim Cl1-O5B \\sim Cl1-O7 \\sim Cl1-O4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim O4 \\sim O7 \\sim O5A \\sim O6A \\sim O6B \\sim O5B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8A) = Uanis(C8B)
Uanis(O6A) = Uanis(O6B)
Uanis(O5A) = Uanis(O5B)
4. Others
 Sof(H9BC)=Sof(H9BD)=Sof(H13A)=Sof(C8B)=Sof(H8B)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(H13)=Sof(C8A)=Sof(H8A)=FVAR(1)
 Sof(O6B)=Sof(O5B)=1-FVAR(2)
 Sof(O5A)=Sof(O6A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C13(H13A), C8A(H8A), C8B(H8B)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9AA,H9AB), C9(H9BC,H9BD), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
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              10250
_olex2_submission_special_instructions 'No special instructions were received'