Chiral and SHG-Active Metal-Organic Frameworks Formed in Solution and on Surfaces: Uniformity, Morphology Control, Oriented Growth, and Post-assembly Functionalization.
Wen, Qiang; Tenenholtz, Shira; Shimon, Linda J. W.; Bar-Elli, Omri; Beck, Lior; Houben, Lothar; Cohen, Sidney R.; Feldman, Yishay; Oron, Dan; Lahav, Michal; van der Boom, Milko E.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c05384

data_4135147
_publ_section_title
;
 Chiral and SHG-Active Metal-Organic Frameworks Formed in Solution and on
 Surfaces: Uniformity, Morphology Control, Oriented Growth, and
 Post-assembly Functionalization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c05384
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C62 H52 Br2 N4 Ni'
_chemical_formula_sum            'C62 H52 Br2 N4 Ni'
_chemical_formula_weight         1071.60
_space_group_crystal_system      hexagonal
_space_group_IT_number           177
_space_group_name_Hall           'P 6 2'
_space_group_name_H-M_alt        'P 6 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   25.8466(8)
_cell_length_b                   25.8466(8)
_cell_length_c                   18.0005(4)
_cell_measurement_reflns_used    4356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.3350
_cell_measurement_theta_min      4.6420
_cell_volume                     10414.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Rigaku XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13662
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        47.899
_diffrn_reflns_theta_max         47.899
_diffrn_reflns_theta_min         3.950
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       'split prism'
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.021
_exptl_transmission_factor_min   0.903
_platon_squeeze_details
;
;
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1006 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0901
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.2583
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                2802
_reflns_number_total             3256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05384_si_002.cif
_cod_data_source_block           v303-sr
_cod_original_cell_volume        10414.1(7)
_cod_database_code               4135147
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.959
_oxdiff_exptl_absorpt_empirical_full_min 0.846
_oxdiff_exptl_absorpt_empirical_full_max 1.223
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              97633
_shelx_hkl_checksum              87210