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_7047969
_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 H26 Fe N10 O4), 4(Cl O4), 3(C3 H6 O)'
_chemical_formula_sum            'C65 H70 Cl4 Fe2 N20 O27'
_chemical_formula_weight         1816.91
_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                110.978(3)
_cell_angle_beta                 95.650(3)
_cell_angle_gamma                91.629(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4649(3)
_cell_length_b                   21.2806(5)
_cell_length_c                   23.1689(8)
_cell_measurement_reflns_used    6544
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      25.2460
_cell_measurement_theta_min      3.5250
_cell_volume                     3868.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -88.00  11.00   1.00   12.00    --  -17.68 -68.00-123.09   99
  2  \w    -88.00  11.00   1.00   12.00    --  -17.68 -68.00 -32.90   99
  3  \w    -89.00  11.00   1.00   12.00    --  -17.68 -69.00  85.76  100
  4  \w    -87.00   8.00   1.00   12.00    --  -17.68 -63.00 164.74   95
  5  \w    -51.00  48.00   1.00   12.00    --   20.00 -67.00-138.90   99
  6  \w    -51.00  48.00   1.00   12.00    --   20.00 -68.00  27.26   99
  7  \w    -51.00  48.00   1.00   12.00    --   20.00 -68.00 102.20   99
  8  \w    -51.00  49.00   1.00   12.00    --   20.00 -69.00 -46.77  100
  9  \w    -51.00  26.00   1.00   12.00    --   20.00 -69.00-166.60   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0070554000
_diffrn_orient_matrix_UB_12      -0.0078110000
_diffrn_orient_matrix_UB_13      0.0274079000
_diffrn_orient_matrix_UB_21      0.0808859000
_diffrn_orient_matrix_UB_22      -0.0065336000
_diffrn_orient_matrix_UB_23      -0.0035272000
_diffrn_orient_matrix_UB_31      0.0230471000
_diffrn_orient_matrix_UB_32      0.0343013000
_diffrn_orient_matrix_UB_33      0.0180597000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.221
_diffrn_reflns_theta_min         3.238
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.560
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         16847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+2.9907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.2041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8370
_reflns_number_total             16847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03511c2.cif
_cod_data_source_block           vg77_5
_cod_depositor_comments
'Adding full bibliography for 7047960--7047970.cif.'
_cod_database_code               7047969
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.798
_reflns_odcompleteness_completeness 99.75
_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. Others
 Fixed Sof: O13(0.5) O14(0.5) O15(0.5) O16(0.5) O17(0.5) O18(0.5) O19(0.5)
 O20(0.5) O21A(0.6) O21B(0.4) O22A(0.6) O22B(0.4) O23A(0.6) O23B(0.4) O24A(0.6)
 O24B(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C27(H27A,H27B), C41(H41A,H41B), C55(H55A,H55B)
3.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),
 C16(H16), C17(H17), C19(H19), C21(H21), C23(H23), C24(H24), C25(H25), C29(H29),
  C30(H30), C31(H31), C33(H33), C35(H35), C37(H37), C38(H38), C39(H39),
 C43(H43), C44(H44), C45(H45), C47(H47), C49(H49), C51(H51), C52(H52), C53(H53)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C42(H42A,H42B,H42C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              80437
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.483