Hierarchy of Supramolecular Arrangements and Building Blocks: Inverted Paradigm of Crystal Engineering in the Unprecedented Metal Coordination of Methylene Blue.
Canossa, Stefano; Bacchi, Alessia; Graiff, Claudia; Pelagatti, Paolo; Predieri, Giovanni; Ienco, Andrea; Manca, Gabriele; Mealli, Carlo; Inorganic chemistry 56 (2017) 3512–3516; doi:10.1021/acs.inorgchem.6b02980

data_4345293
_publ_section_title
;
 Hierarchy of Supramolecular Arrangements and Building Blocks: Inverted
 Paradigm of Crystal Engineering in the Unprecedented Metal Coordination
 of Methylene Blue.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3512
_journal_page_last               3516
_journal_paper_doi               10.1021/acs.inorgchem.6b02980
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'Au Cl2, C16 H18 N3 S'
_chemical_formula_sum            'C16 H18 Au Cl2 N3 S'
_chemical_formula_weight         552.26
_chemical_name_common            'methylene blue gold dichloride'
_chemical_name_systematic        MBAu
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.988(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.281(2)
_cell_length_b                   16.134(4)
_cell_length_c                   14.081(4)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.159
_cell_measurement_theta_min      1.504
_cell_volume                     1808.5(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20508
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.159
_diffrn_reflns_theta_min         1.504
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    8.546
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1367 before and 0.0734 after correction. The Ratio of minimum to maximum transmission is 0.5502. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_preparation
'grinding reacion between methylene blue chloride pentahydrate and gold(I) chloride tetrahydrothiophene'
_exptl_crystal_recrystallization_method
'solvent evaporation from a dichloromethane solution'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.933
_refine_diff_density_min         -2.887
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1621P)^2^+55.9102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3515
_refine_ls_wR_factor_ref         0.3717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2273
_reflns_number_total             3521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02980_si_001.cif
_cod_data_source_block           au3dcm_0m
_cod_depositor_comments
'Adding full bibliography for 4345291--4345293.cif.'
_cod_original_cell_volume        1808.6(8)
_cod_database_code               4345293
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C13(H13), C4(H4), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C1(H1a,H1b,H1c), C15(H15a,H15b,H15c), C2(H2a,H2b,H2c)
;
_shelx_res_checksum              73134
_shelx_hkl_checksum              55396
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'on a glass capillary'
_olex2_submission_original_sample_id MBAu
_olex2_submission_special_instructions 'No special instructions were received'