Langmuir-Blodgett films of salophen-based metallosurfactants as surface pretreatment coatings for corrosion mitigation.
Gonawala, Sunalee; Leopoldino, Verônica R; Kpogo, Kenneth; Verani, Cláudio N; Chemical communications (Cambridge, England) 52 (2016) 11155–11158; doi:10.1039/c6cc04563d

data_7124772
_publ_section_title
;
 Langmuir-Blodgett films of salophen-based metallosurfactants as surface
 pretreatment coatings for corrosion mitigation.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11155
_journal_page_last               11158
_journal_paper_doi               10.1039/c6cc04563d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C42 H59 N2 O7 Zn, C43 H62 N2 O7 Zn, 2(C H4 O)'
_chemical_formula_sum            'C87 H129 N4 O16 Zn2'
_chemical_formula_weight         1617.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-30 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                64.648(6)
_cell_angle_beta                 74.715(7)
_cell_angle_gamma                86.046(7)
_cell_formula_units_Z            2
_cell_length_a                   14.3039(16)
_cell_length_b                   17.603(2)
_cell_length_c                   20.104(2)
_cell_measurement_reflns_used    64892
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      1.8
_cell_volume                     4407.1(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.1334
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78676
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         26.67
_diffrn_reflns_theta_min         1.31
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1734
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.245
_refine_diff_density_max         2.090
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         15386
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1996
_refine_ls_R_factor_gt           0.1384
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3298
_refine_ls_wR_factor_ref         0.3590
_reflns_number_gt                8975
_reflns_number_total             15386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc04563d2.cif
_cod_data_source_block           kksg048_0m-copy
_cod_original_cell_volume        4407.0(9)
_cod_database_code               7124772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O00H-H00H
 0.87 with sigma of 0.01
 C02V-H00H
 1.922654 with sigma of 0.02
 Zn02-H00H
 2.710526 with sigma of 0.02
3.a Rotating group:
 O00O(H00C,H00D)
3.b Secondary CH2 refined with riding coordinates:
 C01K(H01Z,HB), C01X(H3AA,HG), C02C(H02,HJ), C00N(H00A,H00B), C02F(H02G,H02H),
 C02J(H02I,H02J), C013(H01I,H01J)
3.c Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00Z(H00Z), C01C(H01V), C01E(H01W), C01I(H01X), C01N(H01),
 C01S(H1AA), C009(H009), C027(H027), C00L(H00L), C00W(H00W), C01D(H01D),
 C01H(H01H), C01M(H01M), C01T(H01T), C02U(H02U), C023(H023)
3.d Idealised Me refined as rotating group:
 C01J(H01Y,H,HA), C01Q(H0AA,HC,HD), C01V(H2AA,HE,HF), C01Y(H4AA,HH,HI),
 C02E(H5AA,HK,HL), C02H(H6AA,HM,HN), C02I(H7AA,HO,HP), C02K(H8AA,HQ,HR),
 C02L(H9AA,HS,HT), C02M(H0BA,HU,HV), C02P(H1BA,HW,HX), C02Q(H2BA,HY,HZ),
 C024(H3BA,H7BA,H8BA), C025(H4BA,H9BA,H0CA), C01O(H01A,H01B,H01C), C01R(H01E,
 H01F,H01G), C02A(H02A,H02B,H02C), C02B(H02D,H02E,H02F), C02O(H02K,H02L,H02M),
 C02R(H02N,H02O,H02P), C02S(H02Q,H02R,H02S), C02V(H02T,H02V,H02W), C02W(H02X,
 H02Y,H1CA), C02Z(H02Z,H2CA,H3CA), C014(H01K,H01L,H01N), C015(H01O,H01P,H01Q),
 C019(H01R,H01S,H01U), C031(H03A,H03B,H03C), C032(H03D,H03E,H03F), C02T(H5BA,
 H4CA,H5CA), C030(H03G,H03H,H03I)
3.e Idealised tetrahedral OH refined as rotating group:
 O00U(H00U), O01Z(H6BA)
;
_olex2_submission_special_instructions 'No special instructions were received'