Layered 2D Sheetlike Supramolecular Polymers Formed by O–H···Anion Hydrogen Bonds
White, Nicholas G.; Carta, Veronica; MacLachlan, Mark J.; Crystal Growth & Design 15 (2015) 1540–; doi:10.1021/acs.cgd.5b00062

data_4516264
_publ_section_title
;
 Layered 2D Sheetlike Supramolecular Polymers Formed by
 O--H&#x00B7;&#x00B7;&#x00B7;Anion Hydrogen Bonds
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1540
_journal_paper_doi               10.1021/acs.cgd.5b00062
_journal_volume                  15
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C18 H14 O6, C16 H36 N, 0.5(C3 H6 O), Br'
_chemical_formula_sum            'C35.5 H53 Br N O6.5'
_chemical_formula_weight         677.69
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 106.219(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.668(3)
_cell_length_b                   19.384(4)
_cell_length_c                   13.748(3)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.48
_cell_volume                     3497.4(13)
_computing_cell_refinement       'Apex2, (Bruker, 2007)'
_computing_data_collection       'Apex2, (Bruker, 2007)'
_computing_data_reduction        'Apex2, (Bruker, 2007)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27462
_diffrn_reflns_theta_full        27.530
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         1.866
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 7020 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.012(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         15244
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0014842
_refine_ls_shift/su_mean         0.0000348
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.28 6.35 3.14 0.879 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0754
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0754
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              25
_reflns_limit_k_min              -23
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                13244
_reflns_number_total             15290
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      91.11
_oxford_refine_ls_r_factor_ref   0.0369
_oxford_refine_ls_scale          0.101942(14)
_oxford_reflns_number_all        15244
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            cg5b00062_si_002.cif
_cod_data_source_block           3Br
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2020-08-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3497.3(12)
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_moiety     '2(C18 H14 O6), 2(C16 H36 N), C3 H6 O, 2(Br)'
_cod_original_formula_sum        'C71 H106 Br2 N2 O13'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1355.38
_cod_database_code               4516264