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_7062657
_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
'C41.245 H40.491 Cl2 N6 O5 Zn2, 2(F6 P), 0.453(H2 O)'
_chemical_formula_sum            'C41.24 H41.39 Cl2 F12 N6 O5.45 P2 Zn2'
_chemical_formula_weight         1200.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-07-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-15 deposited with the CCDC.	2023-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                77.240(2)
_cell_angle_beta                 69.673(2)
_cell_angle_gamma                72.143(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7082(6)
_cell_length_b                   13.8145(6)
_cell_length_c                   14.4212(6)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      33.12
_cell_measurement_theta_min      2.31
_cell_volume                     2417.44(18)
_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      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0969
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            61834
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.867
_diffrn_source_current           0.93
_diffrn_source_power             0.0465
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1618 before and 0.0968 after correction.
The Ratio of minimum to maximum transmission is 0.8007.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       block
_exptl_crystal_F_000             1213
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.595
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         9010
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+14.3176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6120
_reflns_number_total             9010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02380j2.cif
_cod_data_source_block           at1151_a
_cod_depositor_comments
'Adding full bibliography for 7062656--7062659.cif.'
_cod_database_code               7062657
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.833
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2
 0.89 with sigma of 0.02
 O5A-C42A
 1.42 with sigma of 0.02
 P3-F13 \\sim P3-F14 \\sim P3-F15 \\sim P3-F16 \\sim P3-F17 \\sim P3-F18
 with sigma of 0.01
 F13-F16 \\sim F14-F17 \\sim F15-F18
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(P3) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P2) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim
Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) = Uanis(O5A) = Uanis(C42A)
4. Others
 Sof(O5A)=Sof(H5AA)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(1)
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Sof(O6)=Sof(H6C)=Sof(H6D)=FVAR(2)
 Fixed Sof: P2(0.5) F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) P3(0.5)
 F13(0.5) F14(0.5) F17(0.5) F15(0.5) F18(0.5) F16(0.5)
5.a Free rotating group:
 O6(H6C,H6D)
5.b Rotating group:
 O5(H5A,H5B)
5.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C17(H17), C22(H22), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
  C36(H36), C37(H37), C38(H38), C39(H39)
5.e Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42A(H42A,H42B,H42C)
5.f Idealised tetrahedral OH refined as rotating group:
 O5A(H5AA)
;
_shelx_res_checksum              35886
_olex2_submission_special_instructions 'No special instructions were received'