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_7230173
_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_absolute_configuration unk
_chemical_formula_moiety         'C43 H48 Co Cu2 N4 O6, C3 H6 O, 2(Cl O4)'
_chemical_formula_sum            'C46 H54 Cl2 Co Cu2 N4 O15'
_chemical_formula_weight         1159.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9449(9)
_cell_length_b                   13.2515(6)
_cell_length_c                   19.8004(9)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.515
_cell_measurement_theta_min      2.235
_cell_volume                     5059.7(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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.715
_diffrn_reflns_theta_min         1.865
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0943 before and 0.0487 after correction. The Ratio of minimum to maximum transmission is 0.7074. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.574
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(2)
_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     643
_refine_ls_number_reflns         9017
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0632P)^2^+6.3411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                8247
_reflns_number_total             9017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra13763j2.cif
_cod_data_source_block           3
_cod_original_cell_volume        5059.6(4)
_cod_database_code               7230173
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.415
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(2)
 0.20(2)
2. 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
3. Restrained distances
 O5-H5A = O5-H5B
 0.82 with sigma of 0.01
 C13-C12 \\sim C11-C12 \\sim C11-C10 \\sim C9-C10 \\sim C8-C9 \\sim C13-C8
 with sigma of 0.01
 C33-C32 \\sim C31-C32 \\sim C30-C31 \\sim C30-C29 \\sim C28-C29 \\sim C28-C33
 with sigma of 0.01
 Cl1-O8A \\sim Cl1-O10A \\sim Cl1-O7 \\sim Cl1-O9A
 with sigma of 0.01
 C43-C42 \\sim C42-C41
 with sigma of 0.01
 Cl1-O10A \\sim Cl1A-O10B \\sim Cl1-O9A \\sim Cl1A-O9B \\sim Cl1-O8A \\sim
Cl1A-O8B \\sim Cl1A-O7 ~
 Cl1-O7
 with sigma of 0.01
 Cl2A-O11A \\sim Cl2-O11 \\sim Cl2-O12 \\sim Cl2A-O12A \\sim Cl2-O14 \\sim
Cl2A-O14A \\sim Cl2-O13 ~
 Cl2A-O13A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O9A \\sim O10A \\sim O10B \\sim O9B \\sim O8B \\sim O8A \\sim O7: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl2 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O12A \\sim Cl2A \\sim O11A
\\sim O14A \\sim O13A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C42) = Uanis(C43)
Uanis(C44) = Uanis(C45)
Uanis(C45) = Uanis(C46)
Uanis(O15) = Uanis(C45)
Uanis(O6) = Uanis(C42)
Uanis(Cl1) = Uanis(Cl1A)
Uanis(O9A) = Uanis(O9B)
Uanis(O8A) = Uanis(O8B)
Uanis(O10B) = Uanis(O10A)
Uanis(O14A) = Uanis(O14)
Uanis(O13) = Uanis(O13A)
Uanis(Cl2) = Uanis(Cl2A)
Uanis(O12A) = Uanis(O12)
Uanis(O11) = Uanis(O11A)
5. Others
 Sof(O9B)=Sof(Cl1A)=Sof(O8B)=Sof(O10B)=1-FVAR(1)
 Sof(Cl1)=Sof(O8A)=Sof(O9A)=Sof(O10A)=FVAR(1)
 Sof(O12A)=Sof(Cl2A)=Sof(O11A)=Sof(O14A)=Sof(O13A)=1-FVAR(2)
 Sof(Cl2)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(O14)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C28(H28), C33(H33)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
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), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39)
6.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              57089
_olex2_submission_special_instructions 'No special instructions were received'