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_7047961
_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         'C24 H18 Fe N10 O4, 2(B F4)'
_chemical_formula_sum            'C24 H18 B2 F8 Fe N10 O4'
_chemical_formula_weight         739.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-02
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Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.691(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1725(4)
_cell_length_b                   16.0377(4)
_cell_length_c                   10.6830(3)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.4653
_cell_measurement_theta_min      2.9139
_cell_volume                     2818.22(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_diffrn_measurement_details
;
  1 omega  -88.00    2.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -57.0000    0.0000 90

  2 omega  -88.00    5.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -69.0000  125.8234 93

  3 omega  -88.00    1.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -59.0000 -149.1213 89

  4 omega  -88.00    4.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -68.0000  -78.2451 92

  5 omega  -18.00   45.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       20.8840  -68.0000  151.9306 63

  6 omega  -46.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -68.0000  -87.9211 92

  7 omega  -46.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -68.0000   72.4169 92

  8 omega  -41.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -67.0000  -14.4210 87

  9 omega  -46.00   47.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -69.0000 -149.1086 93

 10 omega  -41.00   49.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340   57.0000 -180.0000 90

 11 omega  -88.00    5.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -69.0000   45.3140 93

 12 omega  -46.00   47.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -69.0000  106.3701 93

 13 omega  -42.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -67.0000  -69.6662 88

 14 omega  -25.00   -3.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -66.0000 -126.6387 22

 15 omega  -43.00   47.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -69.0000   19.2456 90
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
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_diffrn_orient_matrix_UB_11      -0.0256229000
_diffrn_orient_matrix_UB_12      0.0351928000
_diffrn_orient_matrix_UB_13      -0.0040511000
_diffrn_orient_matrix_UB_21      -0.0341680000
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_diffrn_orient_matrix_UB_31      -0.0060035000
_diffrn_orient_matrix_UB_32      -0.0108647000
_diffrn_orient_matrix_UB_33      0.0609032000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            36207
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         2.920
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.744
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.525
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_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0413P)^2^+3.7461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2778
_reflns_number_total             3248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03511c2.cif
_cod_data_source_block           ipc22b077
_cod_depositor_comments
'Adding full bibliography for 7047960--7047970.cif.'
_cod_database_code               7047961
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.969
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_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1A(0.5) H2A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1A), O2(H2A)
;
_shelx_res_checksum              18985
_olex2_submission_special_instructions 'No special instructions were received'