High temperature anionic Fe(III) spin crossover behavior in a mixed-valence Fe(II)/Fe(III) complex.
Ouyang, Zhi-Jian; Mo, Xiao-Ying; Ye, Jia-Qi; Yu, Xiao-Xuan; Huang, Shu-Yuan; Liu, Xiao-Ling; Chen, Wen-Bin; Gao, Song; Dong, Wen; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5960–5967; doi:10.1039/d1dt00111f

data_7707047
_publ_section_title
;
 High temperature anionic Fe(III) spin crossover behavior in a
 mixed-valence Fe(II)/Fe(III) complex.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5960
_journal_page_last               5967
_journal_paper_doi               10.1039/d1dt00111f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C22 H12 Fe N12 O4, C24 H20 P, 2(H2 O)'
_chemical_formula_sum            'C46 H36 Fe N12 O6 P'
_chemical_formula_weight         939.69
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-23 deposited with the CCDC.	2021-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                107.870(2)
_cell_angle_beta                 112.612(2)
_cell_angle_gamma                100.095(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8708(3)
_cell_length_b                   13.1238(3)
_cell_length_c                   15.2393(4)
_cell_measurement_reflns_used    5167
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.8170
_cell_measurement_theta_min      3.4470
_cell_volume                     2131.90(11)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.936
_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    -57.00  28.00   0.50    4.00    --  -47.20  19.00 -90.00  170
  2  \w    -66.00 -29.00   0.50   16.00    -- -102.00 125.00  60.00   74
  3  \w    -58.00  25.00   0.50    4.00    --  -47.20  37.00 150.00  166
  4  \w     -4.00  79.00   0.50    4.00    --   47.20 -96.00 106.00  166
  5  \w     37.00  77.00   0.50   16.00    --  104.75 -96.00 106.00   80
  6  \w     56.00 120.00   0.50   16.00    --  104.75 -61.00  90.00  128
  7  \w     37.00 118.00   0.50   16.00    --  104.75 -45.00 120.00  162
  8  \w     38.00 108.00   0.50   16.00    --  104.75 -94.00  30.00  140
  9  \w     36.00 117.00   0.50   16.00    --  104.75 -45.00 -60.00  162
 10  \w     92.00 142.00   0.50   16.00    --  104.75  96.00-144.00  100
 11  \w    -78.00  12.00   0.50    4.00    --  -47.20  96.00-144.00  180
 12  \w   -106.00 -31.00   0.50   16.00    -- -102.00  96.00-144.00  150
 13  \w   -117.00 -29.00   0.50   16.00    -- -102.00 125.00-120.00  176
 14  \w   -115.00 -79.00   0.50   16.00    -- -102.00 125.00  60.00   72
 15  \w   -116.00 -27.00   0.50   16.00    -- -102.00  15.00  90.00  178
 16  \w   -120.00 -73.00   0.50    4.00    --  -47.20-125.00-120.00   94
 17  \w   -169.00 -74.00   0.50   16.00    -- -102.00-125.00-180.00  190
 18  \w   -144.00 -82.00   0.50   16.00    -- -102.00 -96.00 106.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1018794000
_diffrn_orient_matrix_UB_12      0.0894686000
_diffrn_orient_matrix_UB_13      0.1059307000
_diffrn_orient_matrix_UB_21      -0.0198586000
_diffrn_orient_matrix_UB_22      0.0944906000
_diffrn_orient_matrix_UB_23      -0.0378799000
_diffrn_orient_matrix_UB_31      -0.0902560000
_diffrn_orient_matrix_UB_32      0.0136445000
_diffrn_orient_matrix_UB_33      0.0422477000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19524
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.997
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73660
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0700P)^2^+4.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6314
_reflns_number_total             8336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00111f2.cif
_cod_data_source_block           2018-10-07-5_1
_cod_depositor_comments
'Adding full bibliography for 7707047--7707048.cif.'
_cod_original_cell_volume        2131.90(10)
_cod_database_code               7707047
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe C H O N B'
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.806
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of O5
 At 1.5 times of:
  All O(H) groups, {H7A,H7B} of O7, {H6A,H6B} of O6
2. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O6(0.5) H6A(0.5) H6B(0.5) O7(0.5) H7A(0.5) H7B(0.5)
4.a Riding coordinates:
 O5(H5A,H5B), O7(H7A,H7B)
4.b Free rotating group:
 O6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C7(H7), C8(H8), C10(H10), C15(H15), C16(H16), C18(H18),
 C19(H19), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_shelx_res_checksum              29063
_shelx_hkl_checksum              45457
_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 1.895
_oxdiff_exptl_absorpt_empirical_full_min 0.397