Short- <i>vs</i>. long-range elastic distortion: structural dynamics of a [2 × 2] tetrairon(II) spin crossover grid complex observed by time-resolved X-Ray crystallography.
Velazquez-Garcia, Jose de Jesus; Basuroy, Krishnayan; Storozhuk, Darina; Wong, Joanne; Demeshko, Serhiy; Meyer, Franc; Henning, Robert; Techert, Simone; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt02638d

data_7711634
_publ_section_title
;
 Short- <i>vs</i>. long-range elastic distortion: structural dynamics of a
 [2 \\times 2] tetrairon(II) spin crossover grid complex observed by
 time-resolved X-Ray crystallography.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt02638d
_journal_year                    2022
_chemical_formula_moiety         'C96 H68 Fe4 N24, 4(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C100 H74 B4 F16 Fe4 N26'
_chemical_formula_weight         2210.49
_chemical_properties_physical    Air-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2022-08-06 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.33(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.967(6)
_cell_length_b                   12.821(3)
_cell_length_c                   27.261(5)
_cell_measurement_reflns_used    2916
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.452
_cell_measurement_theta_min      1.791
_cell_volume                     9245(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type
'Standard Huber 515.2 kappa model (APS 14 ID Beamline)'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_number            5237
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.493
_diffrn_reflns_theta_max         25.493
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'undulator radiation'
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'Wavelength normalisation made by Precognition software'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4496
_exptl_crystal_preparation       'Spin crossover'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.346
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         5237
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.308
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.1062
_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^)+(0.1076P)^2^+57.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.2568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4786
_reflns_number_total             5237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02638d2.cif
_cod_data_source_block           fe4_10ns
_cod_database_code               7711634
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.713
_exptl_absorpt_special_details
'Wavelength normalisation process includes the overall absorption and the wavelength-dependent response of the detector'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F6-F7 \\sim F6-F8 \\sim F6-F5 \\sim F7-F8 \\sim F7-F5 \\sim F8-F5
 with sigma of 0.04
 B2-F6 \\sim B2-F7 \\sim B2-F8 \\sim B2-F5
 with sigma of 0.02
 F12-F9 \\sim F12-F10 \\sim F12-F11 \\sim F9-F11 \\sim F10-F11
 with sigma of 0.04
 B3-F12 \\sim B3-F9 \\sim B3-F10 \\sim B3-F11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F6 \\sim B2 \\sim F7 \\sim F8 \\sim F5: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C50 \\sim C49 \\sim N13: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
F10 \\sim B3 \\sim F12 \\sim F9 \\sim F11: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C46, C47, C48, N12, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C42, C41, C40, C39, N11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C36, C35, N9, N10, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, N8, C30, C31, C32, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C29, C28, C27, C26, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C12, C13, C14, N4, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C21, C22, C23, C24, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(B3)=Sof(F12)=Sof(F9)=Sof(F10)=Sof(F11)=1-FVAR(1)
 Sof(F6)=Sof(F7)=Sof(F8)=Sof(F5)=Sof(B2)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C7(H7), C33(H33), C25(H25), C28(H28), C32(H32), C31(H31),
 C18(H18), C16(H16), C48(H48), C24(H24), C4(H4), C2(H2), C8(H8), C3(H3),
 C26(H26), C27(H27), C23(H23), C47(H47), C42(H42), C22(H22), C17(H17), C40(H40),
  C21(H21), C45(H45), C46(H46), C41(H41)
6.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              33623
_shelx_hkl_checksum              7272
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'