Water-Involved Hydrogen Bonds in Dimeric Supramolecular Structures of Magnesium and Zinc Phthalocyaninato Complexes.
Janczak, Jan; ACS omega 4 (2019) 3673–3683; doi:10.1021/acsomega.8b03055

data_4515122
_publ_contact_author
;
    Jan Janczak
    Institute  of Low Temperature and Structure Research 
    Polish Academy of Sciences
    P.O.Box 1410
    Okolna 2 str., 50-950 Wroc\/law
    Poland
;
_publ_section_title
;
 Water-Involved Hydrogen Bonds in Dimeric Supramolecular Structures of
 Magnesium and Zinc Phthalocyaninato Complexes.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              3673
_journal_page_last               3683
_journal_paper_doi               10.1021/acsomega.8b03055
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C32 H18 N8 O Mg, C5 H11 N O'
_chemical_formula_sum            'C37 H29 Mg N9 O2'
_chemical_formula_weight         656.00
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                70.842(11)
_cell_angle_beta                 77.032(12)
_cell_angle_gamma                70.551(14)
_cell_formula_units_Z            2
_cell_length_a                   9.7050(10)
_cell_length_b                   13.171(2)
_cell_length_c                   13.993(2)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.897
_cell_measurement_theta_min      2.951
_cell_volume                     1579.8(4)
_computing_cell_refinement
;
CrysAlis Red 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis CCD 1.171.38.43 (Rigaku Oxford Diffraction, 2015
;
_computing_data_reduction
;
CrysAlis Red 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'KUMA KM-4 with CCD detector'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20497
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.576
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-violet
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      1.375
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7236
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0980P)^2^+0.2070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4195
_reflns_number_total             7236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03055_si_002.cif
_cod_data_source_block           mg4mem
_cod_database_code               4515122
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.975
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              73010
_shelx_hkl_checksum              30802