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_4345292
_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         'C16 H18 Ag Cl2 N3 S'
_chemical_formula_sum            'C16 H18 Ag Cl2 N3 S'
_chemical_formula_weight         463.16
_chemical_name_common            'Methylene blue silver dichloride'
_chemical_name_systematic
'silver(I) 3,7-bis(Dimethylamino)-phenothiazin-5-ium chloride'
_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
_audit_creation_date             2016-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                85.88(3)
_cell_angle_beta                 74.70(3)
_cell_angle_gamma                78.63(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4120(15)
_cell_length_b                   10.468(2)
_cell_length_c                   11.319(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.228
_cell_measurement_theta_min      1.837
_cell_volume                     830.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Pilatus 2M detector'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  template_ELETTRA
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15068
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.228
_diffrn_reflns_theta_min         1.837
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       needle
_exptl_crystal_F_000             464
_exptl_crystal_preparation
'grinding reaction between methylene blue chloride pentaydrate and silver(I)chloride'
_exptl_crystal_recrystallization_method
'solvent evaporation from an acetonitrile solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.911
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0423P)^2^+9.4442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3513
_reflns_number_total             4093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02980_si_001.cif
_cod_data_source_block           merged
_cod_depositor_comments
'Adding full bibliography for 4345291--4345293.cif.'
_cod_database_code               4345292
_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:
 C11(H11), C10(H10), C5(H5), C13(H13), C4(H4), C8(H8)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C15(H15a,H15b,H15c), C2(H2a,H2b,H2c), C16(H16a,H16b,H16c)
;
_shelx_res_checksum              12491
_shelx_hkl_checksum              75464
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-10
_olex2_exptl_crystal_mounting_method 'on a loop, in a Fomblin Y droplet'
_olex2_submission_original_sample_id MBAg
_olex2_submission_special_instructions 'No special instructions were received'