Direct Synthesis of Crystalline Graphdiyne Analogue Based on Supramolecular Interactions.
Zhou, Weixiang; Shen, Han; Wu, Chenyu; Tu, Zeyi; He, Feng; Gu, Yanan; Xue, Yurui; Zhao, Yingjie; Yi, Yuanping; Li, Yongjun; Li, Yuliang; Journal of the American Chemical Society 141 (2019) 48–52; doi:10.1021/jacs.8b09945

data_4133415
_publ_section_title
;
 Direct Synthesis of Crystalline Graphdiyne Analogue Based on
 Supramolecular Interactions.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              48
_journal_page_last               52
_journal_paper_doi               10.1021/jacs.8b09945
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C30 H18, C0.5 H Cl'
_chemical_formula_sum            'C30.5 H19 Cl'
_chemical_formula_weight         420.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
????
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_cell_angle_alpha                90
_cell_angle_beta                 110.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.962(4)
_cell_length_b                   12.826(3)
_cell_length_c                   18.178(4)
_cell_measurement_reflns_used    7128
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4773
_cell_measurement_theta_min      1.1982
_cell_volume                     4569.1(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30554
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.898
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.78630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+6.1563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4956
_reflns_number_total             5232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09945_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        4568.9(18)
_cod_original_formula_sum        'C30.50 H19 Cl'
_cod_database_code               4133415
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H31A(0.5) H31B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
3.c :
 C14(H14), C22(H22), C30(H30)
;
_shelx_res_checksum              49246
_shelx_hkl_checksum              51303
_olex2_submission_special_instructions 'No special instructions were received'