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_7230172
_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         'C40 H44 Cu2 N4 Ni O6, 2(Cl O4)'
_chemical_formula_sum            'C40 H44 Cl2 Cu2 N4 Ni O14'
_chemical_formula_weight         1061.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.497(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9788(6)
_cell_length_b                   23.9304(13)
_cell_length_c                   18.3403(10)
_cell_measurement_reflns_used    7323
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.428
_cell_measurement_theta_min      2.188
_cell_volume                     4816.8(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57816
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_min         1.399
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0909 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.8348. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         9103
_refine_ls_number_restraints     608
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+2.5858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6017
_reflns_number_total             9103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra13763j2.cif
_cod_data_source_block           2
_cod_database_code               7230172
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.846
_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 O(H,H) groups
2. Restrained distances
 C13A-C12A \\sim C13B-C12B \\sim C11A-C12A \\sim C11B-C12B \\sim C11A-C10A
\\sim C10B-C11B \\sim C10B-
 C9B \\sim C10A-C9A \\sim C8B-C9B \\sim C8A-C9A \\sim C13B-C8B \\sim C8A-C13A
 with sigma of 0.01
 Cl1A-O8B \\sim Cl1-O8A \\sim Cl1-O9A \\sim Cl1A-O7B \\sim Cl1-O7A \\sim
Cl1-O10A \\sim Cl1A-O9B ~
 Cl1A-O10B
 with sigma of 0.01
 Cl2-O13 \\sim Cl2A-O13A \\sim Cl2-O14 \\sim Cl2A-O14A \\sim Cl2-O11 \\sim
Cl2A-O11A \\sim Cl2-O12 ~
 Cl2A-O12A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C9A \\sim C12A \\sim C8B \\sim C13A \\sim C10A \\sim C11A \\sim C13B \\sim C8A
\\sim C9B \\sim C10B \\sim C11B \\sim C12B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Cl1 \\sim O7A \\sim O8A \\sim O9A \\sim O10A \\sim O10B \\sim Cl1A \\sim O9B
\\sim O7B \\sim O8B: 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 O13A \\sim Cl2A \\sim O14A
\\sim O11A \\sim O12A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C9A) = Uanis(C9B)
4. Others
 Sof(C8B)=Sof(H8B)=Sof(C13B)=Sof(H13B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=
 Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=
 Sof(H12D)=1-FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C13A)=
 Sof(H13A)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C8A)=
 Sof(H8A)=FVAR(1)
 Sof(O10B)=Sof(Cl1A)=Sof(O9B)=Sof(O7B)=Sof(O8B)=1-FVAR(2)
 Sof(Cl1)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=FVAR(2)
 Sof(O13A)=Sof(Cl2A)=Sof(O14A)=Sof(O11A)=Sof(O12A)=1-FVAR(3)
 Sof(Cl2)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(O14)=FVAR(3)
 Fixed Uiso: H2(0.083) H3(0.1) H4(0.109) H5(0.086) H16(0.084) H17(0.096)
 H18(0.093) H19(0.076) H22(0.089) H23(0.114) H24(0.132) H25(0.111) H27(0.088)
 H28(0.094) H29A(0.115) H29B(0.115) H30A(0.142) H30B(0.142) H31A(0.145)
 H31B(0.145) H32A(0.103) H32B(0.103) H33(0.092) H34(0.079) H36(0.088)
 H37(0.094) H38(0.089) H39(0.075)
 Fixed X: H2(1.28535) H3(1.370589) H4(1.30065) H5(1.15242) H16(0.803741)
 H17(0.876449) H18(1.034699) H19(1.111231) H22(0.95377) H23(0.827921)
 H24(0.63062) H25(0.55969) H27(0.58299) H28(0.698421) H29A(0.475019)
 H29B(0.50466) H30A(0.51573) H30B(0.395) H31A(0.477249) H31B(0.50789)
 H32A(0.67529) H32B(0.7068) H33(0.64636) H34(0.859509) H36(1.03821)
 H37(1.24002) H38(1.346419) H39(1.25351)
 Fixed Y: H2(0.802449) H3(0.716649) H4(0.660801) H5(0.69244) H16(1.08432)
 H17(1.150081) H18(1.127141) H19(1.03811) H22(0.784439) H23(0.720341)
 H24(0.74393) H25(0.83151) H27(0.92282) H28(1.0372) H29A(0.99739) H29B(1.00771)
 H30A(1.103061) H30B(1.08428) H31A(1.09244) H31B(1.14752) H32A(1.113041)
 H32B(1.121351) H33(1.01846) H34(1.08684) H36(1.112081) H37(1.101561)
 H38(1.027861) H39(0.96292)
 Fixed Z: H2(0.76235) H3(0.743) H4(0.64845) H5(0.56977) H16(0.59912)
 H17(0.68008) H18(0.758901) H19(0.763801) H22(0.75529) H23(0.699361)
 H24(0.66483) H25(0.687) H27(0.72327) H28(0.747769) H29A(0.7986) H29B(0.71631)
 H30A(0.73314) H30B(0.76965) H31A(0.881361) H31B(0.839669) H32A(0.91022)
 H32B(0.82789) H33(0.89269) H34(0.9302) H36(0.99227) H37(1.02446) H38(0.977089)
 H39(0.90379)
5.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
5.b Ternary CH refined with riding coordinates:
 C8B(H8B), C13A(H13A), C13B(H13B), C8A(H8A)
5.c Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), C12A(H12A,H12B), C10A(H10A,H10B), C11A(H11A,H11B), C9B(H9BA,
 H9BB), C10B(H10C,H10D), C11B(H11C,H11D), C12B(H12C,H12D)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C14(H14)
;
_shelx_res_checksum              91594
_shelx_fab_checksum              42374
_olex2_submission_special_instructions 'No special instructions were received'