Bifunctional Fe(II) spin crossover-complexes based on ω-(1<i>H</i>-tetrazol-1-yl) carboxylic acids.
Zeni, Willi; Seifried, Marco; Knoll, Christian; Welch, Jan M.; Giester, Gerald; Stöger, Berthold; Artner, Werner; Reissner, Michael; Müller, Danny; Weinberger, Peter; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17183–17193; doi:10.1039/d0dt03315d

data_7706076
_publ_section_title
;
 Bifunctional Fe(II) spin crossover-complexes based on
 \w-(1<i>H</i>-tetrazol-1-yl) carboxylic acids.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17183
_journal_page_last               17193
_journal_paper_doi               10.1039/d0dt03315d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H24 Fe1 N24 O12, 2(B1 F4), 2(C2 H3 N1)'
_chemical_formula_sum            'C22 H30 B2 F8 Fe N26 O12'
_chemical_formula_weight         1080.19
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-08-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.6588(7)
_cell_length_b                   10.6588(7)
_cell_length_c                   34.838(3)
_cell_measurement_reflns_used    1573
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.442
_cell_measurement_theta_min      3.664
_cell_volume                     3427.7(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            22250
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.442
_diffrn_reflns_theta_min         3.664
_exptl_absorpt_coefficient_mu    0.445
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1644
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1573
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0375P)^2^+6.8911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1421
_reflns_number_total             1573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03315d2.cif
_cod_data_source_block           '[Fe(2COOHTz)6](BF4)2_HS'
_cod_original_cell_volume        3427.7(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7706076
_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 O(H) groups
2. Restrained distances
 C4-H4
 0.95 with sigma of 0.01
 C5-H4
 2 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
3.c Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O1(H1A)
;
_shelx_res_checksum              67664
_olex2_submission_special_instructions 'No special instructions were received'