Cooperative 1D Triazole-Based Spin Crossover FeII Material With Exceptional Mechanical Resilience
Pittala, Narsimhulu; Thétiot, Franck; Triki, Smail; Boukheddaden, Kamel; Chastanet, Guillaume; Marchivie, Mathieu; Chemistry of Materials  (2016) –; doi:10.1021/acs.chemmater.6b04118

data_4002697
_publ_section_title
;
 Cooperative 1D Triazole-Based Spin Crossover FeII Material With
 Exceptional Mechanical Resilience
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.6b04118
_journal_year                    2016
_chemical_formula_moiety         'C27 H27 Fe N9, 2(C2 N2 Pt0.5), H2 O'
_chemical_formula_sum            'C31 H29 Fe N13 O Pt'
_chemical_formula_weight         850.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-24
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                95.640(2)
_cell_angle_beta                 101.855(2)
_cell_angle_gamma                92.943(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4945(2)
_cell_length_b                   14.2896(4)
_cell_length_c                   14.8234(4)
_cell_measurement_reflns_used    9224
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.8290
_cell_measurement_theta_min      3.8030
_cell_volume                     1541.93(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -49.00   78.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.5424   77.0000  -90.0000 127

  2 omega  -49.00   78.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.5424   77.0000 -120.0000 127

  3 omega  -14.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2612   77.0000   30.0000 127

  4 omega  -14.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2612   77.0000  150.0000 127

  5 omega  -43.00   50.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.5424   38.0000  120.0000 93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0318604000
_diffrn_orient_matrix_UB_12      -0.0299553000
_diffrn_orient_matrix_UB_13      -0.0419499000
_diffrn_orient_matrix_UB_21      0.0016489000
_diffrn_orient_matrix_UB_22      0.0393908000
_diffrn_orient_matrix_UB_23      -0.0255169000
_diffrn_orient_matrix_UB_31      0.0915689000
_diffrn_orient_matrix_UB_32      -0.0072416000
_diffrn_orient_matrix_UB_33      -0.0031026000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18768
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.370
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       needle
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.2758
_exptl_crystal_size_mid          0.0335
_exptl_crystal_size_min          0.0300
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6308
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5097
_reflns_number_total             6308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm6b04118_si_003.cif
_cod_data_source_block           new120k
_cod_original_cell_volume        1541.93(8)
_cod_database_code               4002697
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 86.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.17
_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 O(H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27)
;
_shelx_res_checksum              77542
_shelx_hkl_checksum              96995
_olex2_submission_special_instructions 'No special instructions were received'