Structure and magnetic characterization of some bicompartmental [N6O2] divalent metal(ii) complexes using bis(phenolato) ligands bearing two pendant bis(pyridyl) amine arms
Mautner, Franz A.; Fischer, Roland C.; Torvisco, Ana; Nakashima, Kai; Handa, Makoto; Mikuriya, Masahiro; Salem, Nahed M. H.; Overby, Gabriel J.; Maier, Madison R.; Louka, Febee R.; Massoud, Salah S.; New Journal of Chemistry 47 (2023) 15638–15649; doi:10.1039/D3NJ02380J

data_7062659
_publ_section_title
;
 Structure and magnetic characterization of some bicompartmental [N6O2]
 divalent metal(ii) complexes using bis(phenolato) ligands bearing two
 pendant bis(pyridyl) amine arms
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15638
_journal_page_last               15649
_journal_paper_doi               10.1039/D3NJ02380J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C39 H34 Cl2 Cu2 N12 O2, 2(H2 O), N O3'
_chemical_formula_sum            'C39 H38 Cl2 Cu2 N13 O7'
_chemical_formula_weight         998.80
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-20 deposited with the CCDC.	2023-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.888(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4530(8)
_cell_length_b                   23.7277(15)
_cell_length_c                   25.4316(16)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.348
_cell_measurement_theta_min      2.377
_cell_volume                     8501.7(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1326
_diffrn_reflns_av_unetI/netI     0.0946
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            141439
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.188
_diffrn_source_current           0.87
_diffrn_source_power             0.0435
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1691 before and 0.0932 after correction.
The Ratio of minimum to maximum transmission is 0.7452.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       Block
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         16649
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0827
_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^)+(0.0295P)^2^+92.3483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11407
_reflns_number_total             16649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02380j2.cif
_cod_data_source_block           rf2461a_0m
_cod_depositor_comments
'Adding full bibliography for 7062656--7062659.cif.'
_cod_database_code               7062659
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.880
_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. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N4) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.02
3.a Free rotating group:
 O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B), C28(H28A,H28B),
 C34(H34A,H34B), C40(H40A,H40B), C47(H47A,H47B), C54(H54A,H54B), C55(H55A,H55B),
  C61(H61A,H61B), C67(H67A,H67B), C73(H73A,H73B), C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
 C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36),
  C37(H37), C38(H38), C39(H39), C44(H44), C46(H46), C51(H51), C53(H53),
 C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64), C65(H65), C66(H66),
  C69(H69), C70(H70), C71(H71), C72(H72), C75(H75), C76(H76), C77(H77),
 C78(H78), C5(H5), C7(H7)
;
_shelx_res_checksum              93317
_olex2_submission_special_instructions 'No special instructions were received'