Spin-crossover compounds based on iron(ii) complexes of 2,6-bis(pyrazol-1-yl)pyridine (bpp) functionalized with carboxylic acid and ethyl carboxylic acid.
García-López, Víctor; Palacios-Corella, Mario; Abhervé, Alexandre; Pellicer-Carreño, Isaac; Desplanches, Cédric; Clemente-León, Miguel; Coronado, Eugenio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16958–16968; doi:10.1039/c8dt03511c

data_7047970
_publ_section_title
;
 Spin-crossover compounds based on iron(ii) complexes of
 2,6-bis(pyrazol-1-yl)pyridine (bpp) functionalized with carboxylic acid
 and ethyl carboxylic acid.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16958
_journal_page_last               16968
_journal_paper_doi               10.1039/c8dt03511c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'2(C28 H28 Fe N10 O4), 2(C28 H26 Fe N10 O4), 3(C3 H6 O), 4(Cl2 O8)'
_chemical_formula_sum            'C121 H126 Cl8 Fe4 N40 O51'
_chemical_formula_weight         3463.61
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-02
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                69.009(4)
_cell_angle_beta                 83.330(4)
_cell_angle_gamma                89.892(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5561(4)
_cell_length_b                   21.3922(9)
_cell_length_c                   23.5484(11)
_cell_measurement_reflns_used    6528
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      22.6340
_cell_measurement_theta_min      3.3640
_cell_volume                     3993.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
  1 omega  -88.00   10.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -67.0000   27.2844 98

  2 omega  -88.00    6.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -57.0000 -180.0000 94

  3 omega  -88.00   11.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -68.0000  -83.9700 99

  4 omega  -89.00   11.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -69.0000  124.1873 100

  5 omega  -52.00   47.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5434  -69.0000 -104.3589 99

  6 omega  -51.00   49.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -69.0000   69.9356 100

  7 omega  -51.00   48.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -68.0000   -6.4472 99

  8 omega  -51.00   49.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -69.0000  175.2479 100

  9 omega  -51.00   15.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5434  -63.0000  134.7372 66
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0090108000
_diffrn_orient_matrix_UB_12      0.0080759000
_diffrn_orient_matrix_UB_13      0.0268699000
_diffrn_orient_matrix_UB_21      -0.0799916000
_diffrn_orient_matrix_UB_22      0.0069718000
_diffrn_orient_matrix_UB_23      -0.0038265000
_diffrn_orient_matrix_UB_31      -0.0223452000
_diffrn_orient_matrix_UB_32      -0.0339079000
_diffrn_orient_matrix_UB_33      0.0178981000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            60459
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       needle
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         17045
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.2250
_refine_ls_R_factor_gt           0.1136
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3075
_refine_ls_wR_factor_ref         0.4051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7004
_reflns_number_total             17045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03511c2.cif
_cod_data_source_block           vg77_4300k77
_cod_depositor_comments
'Adding full bibliography for 7047960--7047970.cif.'
_cod_database_code               7047970
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.804
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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
2. Restrained distances
 Cl4-O22A = Cl4-O23A = Cl4-O22B = Cl4-O24B = Cl4-O24A = Cl4-O21A = Cl4-O23B =
 Cl4-O21B
 1.4 with sigma of 0.02
 Cl5-O26B = Cl5-O28A = Cl5-O27B = Cl5-O25A = Cl5-O26A = Cl5-O28B = Cl5-O25B =
 Cl5-O27A
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O19A \\sim O19B \\sim O18A \\sim O18B \\sim O20A \\sim O20B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O28B \\sim O25B \\sim O26A \\sim O26B \\sim O27A \\sim O27B \\sim O28A \\sim
O25A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O23B \\sim O22A \\sim O22B \\sim O21A \\sim O24B \\sim O23A \\sim O21B \\sim
O24A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: C13A(0.5) H13A(0.5) H13B(0.5) C13B(0.5) H13C(0.5) H13D(0.5)
 C14A(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C14B(0.5) H14D(0.5) H14E(0.5)
 H14F(0.5) C56A(0.5) H56A(0.5) H56B(0.5) C56B(0.5) H56C(0.5) H56D(0.5)
 C57A(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C57B(0.5) H57D(0.5) H57E(0.5)
 H57F(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) H60C(0.5) O29(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C62(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) O30(0.5) C64(0.5) H64A(0.5) H64B(0.5)
 H64C(0.5) C65(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) O31(0.5) O9(0.5)
 O10(0.5) O11(0.5) O12(0.5) O13(0.5) O14(0.5) O15(0.5) O16(0.5) O18A(0.6)
 O18B(0.4) O19A(0.6) O19B(0.4) O20A(0.6) O20B(0.4) O21A(0.6) O21B(0.4)
 O22A(0.6) O22B(0.4) O23A(0.6) O23B(0.4) O24A(0.6) O24B(0.4) O25A(0.6)
 O25B(0.4) O26A(0.6) O26B(0.4) O27A(0.6) O27B(0.4) O28A(0.6) O28B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C16(H16A,H16B), C24(H24A,H24B), C27(H27A,
 H27B), C42(H42A,H42B), C56A(H56A,H56B), C56B(H56C,H56D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C15(H15),
 C17(H17), C19(H19), C21(H21), C23(H23), C25(H25), C29(H29), C30(H30), C31(H31),
  C34(H34), C36(H36), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45),
 C46(H46), C48(H48), C50(H50), C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C14B(H14D,H14E,H14F), C28(H28A,H28B,H28C), C43(H43A,
 H43B,H43C), C57A(H57A,H57B,H57C), C57B(H57D,H57E,H57F), C58(H58A,H58B,H58C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              23800
_olex2_submission_special_instructions 'No special instructions were received'