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_4345291
_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 Cl2 Cu N3 S'
_chemical_formula_sum            'C16 H18 Cl2 Cu N3 S'
_chemical_formula_weight         418.83
_chemical_name_common            'Methylene blue copper dichloride'
_chemical_name_systematic
'copper(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                86.236(6)
_cell_angle_beta                 71.670(6)
_cell_angle_gamma                80.892(5)
_cell_formula_units_Z            2
_cell_length_a                   7.7053(3)
_cell_length_b                   9.9702(7)
_cell_length_c                   11.2564(8)
_cell_measurement_reflns_used    7693
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.2550
_cell_measurement_theta_min      1.8340
_cell_volume                     810.41(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Pilatus 2M detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f      0.00 360.00   0.50    1.00   0.00   0.00   0.00    --   720
;
_diffrn_measurement_device_type  template_ELETTRA
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15861
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.993
_diffrn_reflns_theta_min         1.877
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic orangish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       needle
_exptl_crystal_F_000             428
_exptl_crystal_preparation
'grinding reaction between methylene blue chloride pentahydrate and anhydrous copper (I) chloride'
_exptl_crystal_recrystallization_method
'slow evaporation of a dimethylformamide solution of the grinding product'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.8843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4453
_reflns_number_total             4726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02980_si_001.cif
_cod_data_source_block           mbcu3dmf_1_1_
_cod_depositor_comments
'Adding full bibliography for 4345291--4345293.cif.'
_cod_database_code               4345291
_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:
 C13(H13), C16(H16), C12(H12), C8(H8), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              43155
_shelx_hkl_checksum              30285
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-10
_olex2_exptl_crystal_mounting_method
'on a capton loop, in a Fomblin Y droplet'
_olex2_submission_original_sample_id MBCu
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;