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_7055756
_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 H17 N3 S'
_chemical_formula_sum            'C17 H17 N3 S'
_chemical_formula_weight         295.41
_chemical_name_systematic
'4-ethenylbenzyl N'-[(E)-phenylmethylidene]carbamohydrazonothioate'
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_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                84.169(2)
_cell_angle_beta                 87.2611(19)
_cell_angle_gamma                64.997(2)
_cell_formula_units_Z            2
_cell_length_a                   8.66567(19)
_cell_length_b                   9.3865(3)
_cell_length_c                   10.4897(3)
_cell_measurement_reflns_used    15114
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.4150
_cell_measurement_theta_min      3.1790
_cell_volume                     769.26(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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9921
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_details
;
  1 omega -112.00  -42.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -      -31.8965  160.0000  -35.0000 70

  2 omega  -85.00  -18.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -      -31.8965  118.0000  171.0000 67

  3 omega   50.00  111.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215  160.0000  -35.0000 61

  4 omega   -4.00   85.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215 -118.0000   85.0000 89

  5 omega   21.00  112.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215 -160.0000  -66.0000 91

  6 omega -122.00  -57.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -      -31.8965 -178.0000 -120.0000 65

  7 omega -120.00  -55.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -      -31.8965  178.0000 -180.0000 65

  8 omega  -43.00   59.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215  -38.0000   60.0000 102

  9 omega  -43.00   59.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215  -38.0000  150.0000 102

 10 omega    6.00  108.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215   38.0000 -120.0000 102

 11 omega  -43.00   59.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215  -38.0000  -90.0000 102

 12 omega    3.00  106.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215   57.0000  -60.0000 103

 13 omega    3.00  106.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215   57.0000  150.0000 103

 14 omega   -1.00   63.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215   77.0000 -180.0000 64

 15 omega   -1.00  111.00   1.0000   22.6950
omega____ theta____ kappa____ phi______ frames
    -       32.5215   77.0000   30.0000 112
;
_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      -0.0048627000
_diffrn_orient_matrix_UB_12      0.0654832000
_diffrn_orient_matrix_UB_13      -0.0425682000
_diffrn_orient_matrix_UB_21      0.0112070000
_diffrn_orient_matrix_UB_22      0.0371446000
_diffrn_orient_matrix_UB_23      0.0521835000
_diffrn_orient_matrix_UB_31      0.0894868000
_diffrn_orient_matrix_UB_32      -0.0366206000
_diffrn_orient_matrix_UB_33      -0.0092173000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37171
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         36.31
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77898
_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    1.2753
_exptl_crystal_description       plate
_exptl_crystal_F_000             312.3441
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.4844
_exptl_crystal_size_mid          0.422
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.6580
_refine_diff_density_min         -0.3046
_refine_diff_density_rms         0.0726
_refine_ls_d_res_high            0.6001
_refine_ls_d_res_low             6.8875
_refine_ls_goodness_of_fit_ref   1.0978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    25
_refine_ls_number_parameters     205
_refine_ls_number_reflns         7441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0978
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.2149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6205
_reflns_number_total             7441
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6nj01938b2.cif
_cod_data_source_block           M1_100Kv2
_cod_depositor_comments
'Adding full bibliography for 7055756--7055757.cif.'
_cod_database_code               7055756
_chemical_oxdiff_formula         'C17 H17 N3 S1'
_reflns_odcompleteness_completeness 99.95
_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
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17)
;
_olex2_submission_original_sample_id M1
_olex2_submission_special_instructions 'No special instructions were received'