Toward an Iron(II) Spin-Crossover Grafted Phosphazene Polymer
Ross J. Davidson; Eric W. Ainscough; Andrew M. Brodie; Geoffrey B. Jameson; Mark R. Waterland; Harry R. Allcock; Mark D. Hindenlang; Boujemaa Moubaraki; Keith S. Murray; Keith C. Gordon; Raphael Horvath; Guy N. L. Jameson; Inorganic Chemistry 51 (2012) 8307–8316; doi:10.1021/ic300853f

data_4329877
_publ_contact_author_address
;
 Chemistry-Institute of Fundamental Sciences, Massey University, 
 Private Bag 11222, Palmerston North, New Zealand
;
_publ_contact_author_email       A.M.Brodie@massey.ac.nz
_publ_section_title
;
 Toward an Iron(II) Spin-Crossover Grafted Phosphazene Polymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8307
_journal_page_last               8316
_journal_paper_doi               10.1021/ic300853f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C90 H70 Fe N12 O12 P6, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C92 H73 Cl2 Fe N13 O20 P6'
_chemical_formula_weight         1993.23
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-05-12
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                104.25(3)
_cell_angle_beta                 100.82(3)
_cell_angle_gamma                91.04(3)
_cell_formula_units_Z            2
_cell_length_a                   14.767(3)
_cell_length_b                   16.334(3)
_cell_length_c                   21.024(4)
_cell_measurement_reflns_used    15015
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      69.9
_cell_measurement_theta_min      6.5
_cell_volume                     4816.6(18)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      123.0
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
scan:
    Number of images: 60
               Slice: 20.0000 - 200.0000
         Image width: 3.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 60
               Slice: 20.0000 - 200.0000
         Image width: 3.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 60
               Slice: 20.0000 - 200.0000
         Image width: 3.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 58
               Slice: 22.0000 - 197.0000
         Image width: 3.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 56
               Slice: 22.0000 - 192.0000
         Image width: 3.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 55
               Slice: 20.0000 - 185.0000
         Image width: 3.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.050015
_diffrn_orient_matrix_UB_12      0.033745
_diffrn_orient_matrix_UB_13      -0.010943
_diffrn_orient_matrix_UB_21      0.039255
_diffrn_orient_matrix_UB_22      0.001159
_diffrn_orient_matrix_UB_23      0.044125
_diffrn_orient_matrix_UB_31      0.026307
_diffrn_orient_matrix_UB_32      -0.053595
_diffrn_orient_matrix_UB_33      -0.020828
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38975
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         6.53
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    3.317
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       Block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
C4H10O molecules disordered over several sites and orientations were
found in the unit cell.
The contributions from these were removed using Platon / SQUEEZE.
58 electrons / cell were removed (1.38 C4H10O = 58e-)
and 489.1 A3 was left by the void.
;
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         15495
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                10394
_reflns_number_total             15495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300853f_si_002_2.cif
_cod_data_source_block           rjd314a
_cod_original_cell_volume        4816.6(17)
_cod_original_formula_sum        'C92 H73 Cl2 Fe1 N13 O20 P6 '
_cod_database_code               4329877