Structural Dynamics of Spin Crossover in Iron(II) Complexes with Extended-Tripod Ligands
Stock, P.; Wiedemann, D.; Petzold, H.; Horner, G.; Inorganics 5 (2017) 60–; doi:10.3390/inorganics5030060

data_1556529
_publ_section_title
;
 Structural Dynamics of Spin Crossover in Iron(II) Complexes with
 Extended-Tripod Ligands
;
_journal_name_full               Inorganics
_journal_page_first              60
_journal_paper_doi               10.3390/inorganics5030060
_journal_volume                  5
_journal_year                    2017
_chemical_formula_iupac          '[Zn (C21 H24 N9 P S)](Cl O4)2.1.5C H3 C N'
_chemical_formula_moiety
'C21 H24 N9 P S Zn 2+, 2(Cl O4 1-), 1.5(C2 H3 N)'
_chemical_formula_sum            'C24 H28.5 Cl2 N10.5 O8 P S Zn'
_chemical_formula_weight         791.37
_chemical_name_systematic
; {tris[1-methyl-2-(pyridin-2-ylmethylene-\kN)hydrazinyl-\kN^2^]phosphane
 sulfide}zinc(II) perchlorate--acetonitrile(2/3)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   .
_cell_angle_alpha                90
_cell_angle_beta                 136.39(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0934(12)
_cell_length_b                   31.653(3)
_cell_length_c                   16.281(2)
_cell_measurement_reflns_used    8118
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      31.8740
_cell_measurement_theta_min      3.4640
_cell_volume                     3232.3(19)
_computing_cell_refinement
'CrysAlisPro 1.171.37 (Agilent Technologies, 2014)'
_computing_data_collection
'CrysAlisPro 1.171.37 (Agilent Technologies, 2014)'
_computing_data_reduction
'CrysAlisPro 1.171.37 (Agilent Technologies, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24831
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.37 (Agilent Technologies, 2014)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by Clark and Reid (Clark & Reid, 1995).

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       coloumn
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.4448
_exptl_crystal_size_mid          0.2537
_exptl_crystal_size_min          0.2142
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6322
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0472P)^2^+12.7098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5266
_reflns_number_total             6322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            stock17_final.cif
_cod_data_source_block           stock17
_cod_original_cell_volume        3232.2(12)
_cod_original_formula_sum        'C24 H28.50 Cl2 N10.50 O8 P S Zn'
_cod_database_code               1556529
_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. Uiso/Uaniso restraints and constraints
N50 \\sim C51 \\sim C52: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N30 \\sim C31 \\sim C32: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N40 \\sim C41 \\sim C42: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C42) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N40, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N50(0.5) C51(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) N30(0.5)
 C31(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) N40(0.5) C41(0.5) C42(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5)
5.a Free rotating group:
 N50(C51,C52), N30(C31,C32), N40(C41,C42)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C52(H52A,H52B,H52C),
 C32(H32A,H32B,H32C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'