Tuning of the dimensional linkage from the complex to the framework by thermal conversion in the system Fe/Cl/piperazine.
Schönfeld, F; Wirthensohn, R.; Schmitt, H.-C.; Constantinidis, P.; Fischer, I.; Müller-Buschbaum, K; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15398–15406; doi:10.1039/c4dt01987c

data_7032086
_publ_section_title
;
 Tuning of the dimensional linkage from the complex to the framework by
 thermal conversion in the system Fe/Cl/piperazine.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15398
_journal_page_last               15406
_journal_paper_doi               10.1039/c4dt01987c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C6 H15 Cl2 Fe N3, C2 H4 N'
_chemical_formula_sum            'C8 H20 Cl2 Fe N4'
_chemical_formula_weight         299.03
_chemical_name_systematic        Piperazino-di-chloro-tri-piperazine-iron(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                108.112(6)
_cell_angle_beta                 98.174(6)
_cell_angle_gamma                101.691(6)
_cell_formula_units_Z            2
_cell_length_a                   7.1460(13)
_cell_length_b                   8.3668(16)
_cell_length_c                   11.438(2)
_cell_measurement_reflns_used    4519
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.65
_cell_volume                     620.8(2)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        XPrep
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Microsoft Word (2010)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8074
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.65
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6356
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0891 before and 0.0356 after correction.
The Ratio of minimum to maximum transmission is 0.8528.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.9093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2281
_reflns_number_total             2515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01987c2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7032085--7032087.cif.'
_cod_database_code               7032086
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3), N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C7(H7A,H7B), C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B),
 C8(H8A,H8B), C6(H6A,H6B)
;