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_7706081
_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         'C30 H48 Fe N24 O12, 2(Cl O4), C4 H10 O'
_chemical_formula_sum            'C34 H58 Cl2 Fe N24 O21'
_chemical_formula_weight         1265.79
_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   geom
_audit_creation_date             2020-08-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-21 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                96.080(4)
_cell_angle_beta                 93.160(4)
_cell_angle_gamma                116.571(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6262(13)
_cell_length_b                   11.0192(13)
_cell_length_c                   27.044(3)
_cell_measurement_reflns_used    6899
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      23.434
_cell_measurement_theta_min      2.204
_cell_volume                     2797.5(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            61136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         2.089
_exptl_absorpt_coefficient_mu    0.459
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1316
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         13866
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0874
_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^)+(0.0902P)^2^+9.4631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6407
_reflns_number_total             13866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03315d2.cif
_cod_data_source_block           '[Fe(4COOHTz)6](ClO4)2_HS'
_cod_database_code               7706081
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6A,H6B,H6C} of C6, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H9A,H9B,H9C} of C9
2. Restrained distances
 O2C-H2C
 1 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C2A(H2AA,H2AB), C2B(H2BA,H2BB), C4(H4A,H4B),
 C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4A(H4AA,H4AB), C4B(H4BA,H4BB), C2C(H2CA,H2CB),
  C2D(H2DA,H2DB), C2E(H2EA,H2EB), C3C(H3CA,H3CB), C3D(H3DA,H3DB), C3E(H3EA,
 H3EB), C4C(H4CA,H4CB), C4D(H4DA,H4DB), C4E(H4EA,H4EB), C7(H7A,H7B), C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1C), C1A(H1AA), C1B(H1BA), C1C(H1CA), C1D(H1DA), C1E(H1EA)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
3.d Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O1(H1), O1A(H1A), O1B(H1B), O1D(H1D), O1E(H1E), O2C(H2C)
;
_shelx_res_checksum              2874
_olex2_submission_special_instructions 'No special instructions were received'