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_7230168
_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 H42 Cu3 N4 O5, 2(Cl O4)'
_chemical_formula_sum            'C40 H42 Cl2 Cu3 N4 O13'
_chemical_formula_weight         1048.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_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                89.031(8)
_cell_angle_beta                 80.648(8)
_cell_angle_gamma                80.267(8)
_cell_formula_units_Z            2
_cell_length_a                   10.021(2)
_cell_length_b                   13.993(3)
_cell_length_c                   15.997(4)
_cell_measurement_reflns_used    1979
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.261
_cell_measurement_theta_min      2.518
_cell_volume                     2181.4(8)
_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 0.996
_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  0.1060
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25662
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.290
_exptl_absorpt_coefficient_mu    1.640
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0990 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.7254. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7658
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1004P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3983
_reflns_number_total             7658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra13763j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2181.3(8)
_cod_database_code               7230168
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 Fixed Uiso: H2(0.07) H3(0.078) H4(0.082) H5(0.071) H7(0.075) H8(0.084)
 H9A(0.078) H9B(0.078) H10A(0.107) H10B(0.107) H11A(0.133) H11B(0.133)
 H12A(0.079) H12B(0.079) H13(0.112) H14(0.077) H16(0.075) H17(0.073) H18(0.071)
 H19(0.067) H22(0.069) H23(0.079) H24(0.085) H25(0.074) H27(0.081) H28(0.097)
 H29A(0.099) H29B(0.099) H30A(0.143) H30B(0.143) H31A(0.122) H31B(0.122)
 H32A(0.08) H32B(0.08) H33(0.092) H34(0.067) H36(0.071) H37(0.089) H38(0.082)
 H39(0.071) H5A(0.1) H5B(0.1)
 Fixed X: H2(0.658891) H3(0.83966) H4(0.821441) H5(0.62049) H7(0.40346)
 H8(0.111641) H9A(0.249449) H9B(0.21563) H10A(-0.00668) H10B(0.06614)
 H11A(0.004539) H11B(-0.12488) H12A(-0.11512) H12B(-0.07842) H13(0.14009) H14(-
 0.08432) H16(-0.19437) H17(-0.20906) H18(-0.027651) H19(0.165661) H22(0.36023)
 H23(0.3804) H24(0.54016) H25(0.67586) H27(0.74848) H28(0.83593) H29A(0.76972)
 H29B(0.899341) H30A(0.99368) H30B(0.949499) H31A(0.774089) H31B(0.900789)
 H32A(0.824409) H32B(0.69589) H33(0.614181) H34(0.611921) H36(0.52614)
 H37(0.435529) H38(0.36303) H39(0.37115) H5A(0.17099) H5B(0.254769)
 Fixed Y: H2(0.60881) H3(0.55885) H4(0.442509) H5(0.381881) H7(0.368281)
 H8(0.432889) H9A(0.24436) H9B(0.31412) H10A(0.3029) H10B(0.196529)
 H11A(0.19948) H11B(0.249749) H12A(0.39544) H12B(0.32427) H13(0.32499)
 H14(0.46952) H16(0.574519) H17(0.69589) H18(0.777829) H19(0.7408) H22(0.73632)
 H23(0.79569) H24(0.89295) H25(0.935559) H27(0.936249) H28(0.86969)
 H29A(1.05817) H29B(0.981509) H30A(0.989349) H30B(1.09697) H31A(1.118521)
 H31B(1.07006) H32A(0.926439) H32B(1.00521) H33(0.99976) H34(0.87007)
 H36(0.775009) H37(0.64291) H38(0.54176) H39(0.58154) H5A(0.812261)
 H5B(0.860701)
 Fixed Z: H2(0.20728) H3(0.10089) H4(0.001141) H5(0.01039) H7(0.07038)
 H8(0.13516) H9A(0.12252) H9B(0.04817) H10A(0.07284) H10B(0.08337)
 H11A(0.21688) H11B(0.18048) H12A(0.23298) H12B(0.305861) H13(0.27166)
 H14(0.36293) H16(0.473539) H17(0.568951) H18(0.565221) H19(0.46258)
 H22(0.12779) H23(-0.00714) H24(-0.0537) H25(0.0385) H27(0.16993) H28(0.33708)
 H29A(0.275599) H29B(0.239909) H30A(0.361171) H30B(0.335409) H31A(0.43532)
 H31B(0.475639) H32A(0.49127) H32B(0.52341) H33(0.4015) H34(0.55333)
 H36(0.663151) H37(0.71404) H38(0.623711) H39(0.482229) H5A(0.263901)
 H5B(0.298181)
;
_shelx_res_checksum              28613
_shelx_fab_checksum              20424
_olex2_submission_special_instructions 'No special instructions were received'