Elucidating the Growth of Metal-Organic Nanotubes Combining Isoreticular Synthesis with Liquid-Cell Transmission Electron Microscopy.
Vailonis, Kristina M.; Gnanasekaran, Karthikeyan; Powers, Xian B.; Gianneschi, Nathan C.; Jenkins, David M.; Journal of the American Chemical Society 141 (2019) 10177–10182; doi:10.1021/jacs.9b04586

data_4128047
_publ_section_title
;
 Elucidating the Growth of Metal-Organic Nanotubes Combining Isoreticular
 Synthesis with Liquid-Cell Transmission Electron Microscopy.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10177
_journal_page_last               10182
_journal_paper_doi               10.1021/jacs.9b04586
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C8 H6 Br Cu N3'
_chemical_formula_sum            'C8 H6 Br Cu N3'
_chemical_formula_weight         287.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.374(3)
_cell_length_b                   6.9783(8)
_cell_length_c                   13.2425(15)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      3.21
_cell_volume                     2067.6(4)
_computing_cell_refinement       'SAINT V8.37A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.37A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 2 CMOS detector'
_diffrn_measurement_method       '\w/\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24015
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         32.507
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'Beamline 12.2.1, ALS'
_exptl_absorpt_coefficient_mu    6.317
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.793
_refine_diff_density_min         -2.788
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1511P)^2^+7.8720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2193
_refine_ls_wR_factor_ref         0.2360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1487
_reflns_number_total             1908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04586_si_002.cif
_cod_data_source_block           xbp211
_cod_database_code               4128047
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.543
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              38753
_shelx_hkl_checksum              74462