Magnetic nanoparticles with chelating shells prepared by RAFT/MADIX polymerization
Markiewicz, Karolina H.; Zembko, Paula; Półtorak, Katarzyna; Misztalewska, Iwona; Wojtulewski, Sławomir; Majcher, Anna M.; Fornal, Emilia; Wilczewska, Agnieszka Z.; New J. Chem. 40 (2016) 9223–; doi:10.1039/C6NJ01938B

data_7055757
_publ_section_title
;
 Magnetic nanoparticles with chelating shells prepared by RAFT/MADIX
 polymerization
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9223
_journal_paper_doi               10.1039/C6NJ01938B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C17 H18 N3 S, C H4 O, Cl'
_chemical_formula_sum            'C18 H22 Cl N3 O S'
_chemical_formula_weight         363.90
_chemical_name_systematic
'(1E,2E)-1-{amino[(4-ethenylbenzyl)sulfanyl]methylidene}-2-benzylidenehydrazinium chloride - methanol (1:1:1)'
_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             2015-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2015-02-16 deposited with the CCDC.
2016-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                67.799(2)
_cell_angle_beta                 68.787(2)
_cell_angle_gamma                66.310(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4176(2)
_cell_length_b                   10.2256(2)
_cell_length_c                   11.8640(3)
_cell_measurement_reflns_used    13960
_cell_measurement_temperature    100.1(6)
_cell_measurement_theta_max      36.9700
_cell_measurement_theta_min      3.3560
_cell_volume                     938.48(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -61.00   42.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -      -31.5329   57.0000  -90.0000 103

  2 omega  -61.00   42.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -      -31.5329   57.0000  -30.0000 103

  3 omega   -1.00  111.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   77.0000    0.0000 112

  4 omega   -1.00  111.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   77.0000   60.0000 112

  5 omega    3.00  106.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   57.0000  150.0000 103

  6 omega   -1.00  111.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   77.0000 -150.0000 112

  7 omega    3.00  106.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   57.0000  -60.0000 103

  8 omega   -1.00  111.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   77.0000 -180.0000 112

  9 omega   -1.00  111.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -       32.1579   77.0000  -30.0000 112

 10 omega  -65.00   47.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -      -31.5329   77.0000   30.0000 112

 11 omega  -65.00   44.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -      -31.5329   77.0000 -180.0000 109

 12 omega  -61.00   42.00   1.0000   27.1850
omega____ theta____ kappa____ phi______ frames
    -      -31.5329   57.0000  120.0000 103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      -0.0561667000
_diffrn_orient_matrix_UB_12      0.0071129000
_diffrn_orient_matrix_UB_13      -0.0304502000
_diffrn_orient_matrix_UB_21      0.0485267000
_diffrn_orient_matrix_UB_22      0.0280819000
_diffrn_orient_matrix_UB_23      -0.0589767000
_diffrn_orient_matrix_UB_31      0.0411974000
_diffrn_orient_matrix_UB_32      -0.0731994000
_diffrn_orient_matrix_UB_33      -0.0060650000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45409
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.2984
_exptl_crystal_size_mid          0.2133
_exptl_crystal_size_min          0.0934
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         9081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.3447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                6918
_reflns_number_total             9081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj01938b2.cif
_cod_data_source_block           exp_2220
_cod_depositor_comments
'Adding full bibliography for 7055756--7055757.cif.'
_cod_original_cell_volume        938.49(4)
_cod_database_code               7055757
_chemical_oxdiff_formula         'C18 H22 N3 S1 Cl1 O1'
_chemical_oxdiff_usercomment     100K
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14),
  C15(H15), C16(H16), C17(H17)
2.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_olex2_submission_original_sample_id M2
_olex2_submission_special_instructions 'No special instructions were received'