Synthesis-dependent properties of barlowite and Zn-substituted barlowite
Smaha, Rebecca W.; He, Wei; Sheckelton, John P.; Wen, Jiajia; Lee, Young S.; Journal of Solid State Chemistry 268 (2018) 123–129; doi:10.1016/j.jssc.2018.08.016

data_1560771
_publ_section_title
;
 Synthesis-dependent properties of barlowite and Zn-substituted barlowite
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              123
_journal_page_last               129
_journal_paper_doi               10.1016/j.jssc.2018.08.016
_journal_volume                  268
_journal_year                    2018
_chemical_formula_moiety         '1(Br1), Cu3.67 H6 O6 Zn0.33, 1(F1)'
_chemical_formula_sum            'Br Cu3.67 F H6 O6 Zn0.34'
_chemical_formula_weight         455.73
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   6.6680(4)
_cell_length_b                   6.6680(4)
_cell_length_c                   9.3036(6)
_cell_measurement_reflns_used    5358
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.255
_cell_measurement_theta_min      2.414
_cell_volume                     358.24(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         24.411
_diffrn_reflns_theta_min         2.051
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.928
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.7492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1357 before and 0.1034 after correction. The Ratio 
of minimum to maximum transmission is 0.7818. The \l/2 correction 
factor is Not present.'
;
_exptl_crystal_colour            'clear bluish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    4.225
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             429
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.336
_refine_ls_extinction_coef       0.062(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         614
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0345P)^2^+0.1910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                556
_reflns_number_total             614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-268-123.cif
_cod_data_source_block           'data_Zn-2disorder_RS109'
_cod_original_cell_volume        358.24(5)
_cod_original_formula_sum        'Br Cu3.67 H6 F O6 Zn0.34'
_cod_database_code               1560771
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All Zn(H) groups
2. Shared sites
{Cu2, Zn1}
3. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cu2) = Uanis(Zn1)
5. Others
 Fixed Sof: Zn1(0.02778) Cu2(0.05556)
;
_shelx_res_checksum              59953
_shelx_hkl_checksum              45699