New salicylaldoximato-borate ligands resulting from anion hydrolysis and their respective copper and iron complexes.
Woodhouse, Sidney S.; De Silva, D Nirosha T; Jameson, Geoffrey B.; Cutler, Daniel J.; Sanz, Sergio; Brechin, Euan K.; Davies, Casey G.; Jameson, Guy N. L.; Plieger, Paul G.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11872–11881; doi:10.1039/c9dt01968e

data_7700503
_publ_section_title
;
 New salicylaldoximato-borate ligands resulting from anion hydrolysis and
 their respective copper and iron complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11872
_journal_page_last               11881
_journal_paper_doi               10.1039/c9dt01968e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C66 H76 B Fe3 N10 O12, 2(B F4), 2(H2 O), 2(C5 H5 N)'
_chemical_formula_sum            'C76 H90 B3 F8 Fe3 N12 O14'
_chemical_formula_weight         1747.57
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-02 deposited with the CCDC.    2019-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.408(5)
_cell_length_b                   19.133(5)
_cell_length_c                   30.848(5)
_cell_measurement_reflns_used    709
_cell_measurement_temperature    143
_cell_measurement_theta_max      45.6
_cell_measurement_theta_min      6.8
_cell_volume                     9094(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_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      143.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
scan:
    Number of images: 60
               Slice: 20.0000 - 170.0000
         Image width: 2.5000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 70
               Slice: 24.0000 - 199.0000
         Image width: 2.5000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 62
               Slice: 21.0000 - 176.0000
         Image width: 2.5000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 42
               Slice: 47.0000 - 152.0000
         Image width: 2.5000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Loop
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1248
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            57601
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        58.931
_diffrn_reflns_theta_max         58.931
_diffrn_reflns_theta_min         6.824
_exptl_absorpt_coefficient_mu    4.457
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Chip
_exptl_crystal_F_000             3628
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         6442
_refine_ls_number_restraints     671
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0861
_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^)+(0.1731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2471
_refine_ls_wR_factor_ref         0.2674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4575
_reflns_number_total             6442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01968e1.cif
_cod_data_source_block           c2
_cod_depositor_comments
'Adding full bibliography for 7700501--7700503.cif.'
_cod_database_code               7700503
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.518
_shelx_estimated_absorpt_t_min   0.131
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F8)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(B1) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(B3) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C102) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C110) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: B2(0.5) F2(0.5) F4(0.5) F3(0.5) F1(0.5) B3(0.5) F5(0.5) F7(0.5)
 F6(0.5) F8(0.5) C102(0.5) H102(0.5) C101(0.5) H101(0.5) N100(0.5) C105(0.5)
 H105(0.5) C104(0.5) H104(0.5) C103(0.5) H103(0.5) C107(0.5) H107(0.5)
 C108(0.5) H108(0.5) C109(0.5) H109(0.5) C110(0.5) H110(0.5) C111(0.5)
 H111(0.5) N106(0.5)
5.a Riding coordinates:
 O3(H3)
5.b Free rotating group:
 B2(F2,F4,F3,F1), B3(F5,F7,F6,F8), O1W(H1WA,H1WB), C102(C101,N100,C105,C104,
 C103)
5.c Ternary CH refined with riding coordinates:
 N622(H622), N612(H612)
5.d Secondary CH2 refined with riding coordinates:
 C621(H62A,H62B), C624(H62F,H62G), C614(H61A,H61B), C611(H61C,H61D)
5.e Me refined with riding coordinates:
 C421(H42A,H42B,H42C), C623(H62C,H62D,H62E), C411(H41A,H41B,H41C), C613(H61E,
 H61F,H61G)
5.f Aromatic/amide H refined with riding coordinates:
 C52(H52), C32(H32), C221(H221), C626(H626), C616(H616), C617(H617),
 C618(H618), C31(H31), C51(H51), C28(H28), C29(H29), C30(H30), C1AA(H1AA),
 C3AA(H3AA), C211(H211), C102(H102), C101(H101), C105(H105), C104(H104),
 C103(H103), C107(H107), C108(H108), C109(H109), C110(H110), C111(H111)
5.g Fitted hexagon refined as free rotating group:
 C107(C108,C109,C110,C111,N106)
;
_shelx_res_checksum              51356
_shelx_fab_checksum              28932
_olex2_submission_special_instructions 'No special instructions were received'