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_7700501
_publ_section_title
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 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
'C52 H68 B2 F2 Fe2 N8 O14, 4(C H4 O), 2(B F4)'
_chemical_formula_sum            'C56 H84 B4 F10 Fe2 N8 O18'
_chemical_formula_weight         1502.25
_chemical_properties_physical    Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-03 deposited with the CCDC.    2019-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                73.437(5)
_cell_angle_beta                 71.084(3)
_cell_angle_gamma                67.319(5)
_cell_formula_units_Z            1
_cell_length_a                   10.292(5)
_cell_length_b                   12.325(3)
_cell_length_c                   15.431(5)
_cell_measurement_reflns_used    14422
_cell_measurement_temperature    152
_cell_measurement_theta_max      71.7
_cell_measurement_theta_min      6.7
_cell_volume                     1679.5(11)
_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      152.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23554
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         72.048
_diffrn_reflns_theta_min         6.693
_exptl_absorpt_coefficient_mu    4.352
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       Block
_exptl_crystal_F_000             782
_exptl_crystal_preparation       Mossbauer
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          1.01
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0542P)^2^+1.9589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5713
_reflns_number_total             6229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01968e1.cif
_cod_data_source_block           c1
_cod_depositor_comments
'Adding full bibliography for 7700501--7700503.cif.'
_cod_database_code               7700501
_shelx_shelxl_version_number     2018/3
_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
2. Restrained distances
 F4-B1B \\sim F4'-B1B \\sim F3B-B1B \\sim F1-B1B \\sim F1'-B1B \\sim F2-B1B
 with sigma of 0.02
 F4-B1A \\sim F1-B1A \\sim F3B-B1B \\sim F4'-B1B \\sim F1'-B1B \\sim F2-B1B
\\sim F2-B1A \\sim F3A-B1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(B1B) = Uanis(B1A)
4. Others
 Sof(B1B)=Sof(F1')=Sof(F3B)=Sof(F4')=1-FVAR(1)
 Sof(F1)=Sof(F4)=Sof(F3A)=Sof(B1A)=FVAR(1)
5.a Rotating group:
 421(HA,HB,HC), C411(H41A,H41B,H41C)
5.b Secondary CH2 refined with riding coordinates:
 C621(H62A,H62B), C627(H62C,H62D), C626(H62E,H62F), C624(H62G,H62H), C623(H62I,
 H62J), C611(H61A,H61B), C613(H61C,H61D), C614(H61E,H61F), C616(H61G,H61H),
 C617(H61I,H61J)
5.c Aromatic/amide H refined with riding coordinates:
 C52(H52), C32(H32), C221(H221), C15(H15), C31(H31), C211(H211)
5.d Idealised Me refined as rotating group:
 C702(H70A,H70B,H70C), C701(H70D,H70E,H70F)
5.e Idealised tetrahedral OH refined as rotating group:
 O701(H701)
;
_shelx_res_checksum              64934
_olex2_submission_special_instructions 'No special instructions were received'