Hydrocarbon Belts with Truncated Cone Structures.
Zhang, Qian; Zhang, Yan-E; Tong, Shuo; Wang, Mei-Xiang; Journal of the American Chemical Society 142 (2020) 1196–1199; doi:10.1021/jacs.9b12181

data_4134118
_publ_section_title
;
 Hydrocarbon Belts with Truncated Cone Structures.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1196
_journal_page_last               1199
_journal_paper_doi               10.1021/jacs.9b12181
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C48 H48, C H3 N O2'
_chemical_formula_sum            'C49 H51 N O2'
_chemical_formula_weight         725.86
_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             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.846(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8553(4)
_cell_length_b                   12.3832(3)
_cell_length_c                   37.1996(8)
_cell_measurement_reflns_used    5404
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.2860
_cell_measurement_theta_min      4.4930
_cell_volume                     7746.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -120.00 -68.00   0.50    0.30    --  -47.20-130.00  44.00  104
  2  \w   -120.00 -62.00   0.50    0.30    --  -47.20-139.00-130.00  116
  3  \w     74.00 120.00   0.50    0.30    --   47.20 130.00 115.00   92
  4  \w     24.00 103.00   0.50    0.30    --   47.20-139.00-130.00  158
  5  \w     19.00  97.00   0.50    0.30    --   47.20-130.00  44.00  156
  6  \w   -168.00 -62.00   0.50    1.00    --  -99.00-139.00-130.00  212
  7  \w     31.00 121.00   0.50    1.00    --  103.25-130.00  44.00  180
  8  \w     31.00 127.00   0.50    1.00    --  103.25-139.00-130.00  192
  9  \w     74.00 169.00   0.50    1.00    --  103.25 130.00 115.00  190
 10  \w   -120.00 -71.00   0.50    0.30    --  -47.20-125.00  90.00   98
 11  \w   -102.00 -18.00   0.50    0.30    --  -47.20 139.00 -69.00  168
 12  \w   -119.00 -77.00   0.50    0.30    --  -47.20-125.00-120.00   84
 13  \w     26.00 118.00   0.50    0.30    --   47.20  77.00 120.00  184
 14  \w   -167.00 -86.00   0.50    1.00    --  -99.00 -45.00 -60.00  162
 15  \w   -115.00 -26.00   0.50    1.00    --  -99.00  61.00 150.00  178
 16  \w     92.00 111.50   0.50    1.00    --  103.25  45.00 120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0177392000
_diffrn_orient_matrix_UB_12      0.0224483000
_diffrn_orient_matrix_UB_13      0.0404685000
_diffrn_orient_matrix_UB_21      -0.0060666000
_diffrn_orient_matrix_UB_22      0.1222968000
_diffrn_orient_matrix_UB_23      -0.0072603000
_diffrn_orient_matrix_UB_31      -0.0896514000
_diffrn_orient_matrix_UB_32      -0.0038093000
_diffrn_orient_matrix_UB_33      0.0057331000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            29943
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.633
_diffrn_reflns_theta_min         2.381
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       prism
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1335P)^2^+19.9942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5212
_reflns_number_total             7129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_004.cif
_cod_data_source_block           tx189
_cod_depositor_comments
;

2020-08-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '0.07(C48 H48), 0.07(C H3 N O2)'
_cod_original_formula_sum        'C3.63 H3.78 N0.07 O0.15'
_cod_original_formula_units_Z    108
_cod_original_formula_weight     50.81
_cod_database_code               4134118
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCl
_reflns_odcompleteness_completeness 96.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H001(0.028) H002(0.028) H003(0.027) H007(0.033) H00A(0.032)
 H00C(0.031) H00D(0.03) H00G(0.034) H00B(0.032) H00E(0.032) H00J(0.032)
 H00F(0.034) H00H(0.034) H00M(0.031) H00O(0.036) H00Q(0.032) H00I(0.036)
 H00K(0.036) H00U(0.035) H00V(0.037) H00W(0.035) H00Z(0.035) H01A(0.042)
 H01B(0.042) H011(0.039) H012(0.044) H01C(0.044) H01D(0.044) H01E(0.045)
 H01F(0.045) H015(0.039) H016(0.043) H01G(0.047) H01H(0.047) H01I(0.07)
 H01J(0.07) H01K(0.07) H01L(0.081) H01M(0.081) H01N(0.081) H01O(0.055)
 H01P(0.055) H01W(0.076) H01X(0.076) H01Y(0.076) H01Q(0.09) H01R(0.09)
 H01S(0.09) H01T(0.103) H01U(0.103) H01V(0.103)
 Fixed X: H001(0.340864) H002(0.37027) H003(0.480603) H007(0.177745)
 H00A(0.148826) H00C(0.272047) H00D(0.197209) H00G(0.414836) H00B(0.433245)
 H00E(0.484655) H00J(0.346307) H00F(0.263609) H00H(0.197067) H00M(0.296284)
 H00O(0.035082) H00Q(0.435101) H00I(0.262999) H00K(0.301448) H00U(-0.01287)
 H00V(0.191214) H00W(-0.014122) H00Z(0.069075) H01A(0.135993) H01B(0.059477)
 H011(0.270713) H012(-0.100269) H01C(0.58534) H01D(0.535039) H01E(0.381761)
 H01F(0.420347) H015(0.148647) H016(-0.08066) H01G(0.285297) H01H(0.352021)
 H01I(0.363973) H01J(0.277428) H01K(0.344578) H01L(0.597527) H01M(0.551651)
 H01N(0.635647) H01O(0.073119) H01P(0.003035) H01W(0.370947) H01X(0.281941)
 H01Y(0.308094) H01Q(0.458114) H01R(0.411259) H01S(0.368623) H01T(0.160944)
 H01U(0.09422) H01V(0.088727)
 Fixed Y: H001(0.578795) H002(0.854602) H003(0.693027) H007(0.890392)
 H00A(0.612427) H00C(1.101444) H00D(0.377188) H00G(0.62032) H00B(0.709418)
 H00E(0.612399) H00J(0.95765) H00F(0.516387) H00H(0.432829) H00M(0.495616)
 H00O(1.011798) H00Q(0.795345) H00I(1.049741) H00K(0.93837) H00U(0.553843)
 H00V(0.353924) H00W(0.785146) H00Z(0.379916) H01A(0.760025) H01B(0.700272)
 H011(1.128622) H012(0.713241) H01C(0.739912) H01D(0.830203) H01E(1.137557)
 H01F(1.025906) H015(1.149899) H016(0.888685) H01G(0.292711) H01H(0.380585)
 H01I(0.289911) H01J(0.324515) H01K(0.411768) H01L(0.650505) H01M(0.745888)
 H01N(0.76596) H01O(0.928267) H01P(0.862094) H01W(0.276953) H01X(0.302874)
 H01Y(0.183559) H01Q(1.080366) H01R(0.971039) H01S(1.079432) H01T(0.859641)
 H01U(0.785349) H01V(0.911005)
 Fixed Z: H001(0.392317) H002(0.394364) H003(0.338357) H007(0.422516)
 H00A(0.421052) H00C(0.381222) H00D(0.376319) H00G(0.258538) H00B(0.409434)
 H00E(0.397251) H00J(0.275105) H00F(0.430234) H00H(0.437949) H00M(0.271919)
 H00O(0.320712) H00Q(0.260249) H00I(0.441579) H00K(0.43315) H00U(0.318113)
 H00V(0.29012) H00W(0.414876) H00Z(0.307068) H01A(0.452133) H01B(0.463122)
 H011(0.294412) H012(0.336556) H01C(0.383221) H01D(0.40062) H01E(0.429937)
 H01F(0.421387) H015(0.312198) H016(0.336043) H01G(0.420791) H01H(0.419608)
 H01I(0.474502) H01J(0.482477) H01K(0.481235) H01L(0.439327) H01M(0.456309)
 H01N(0.441851) H01O(0.465279) H01P(0.480189) H01W(0.178989) H01X(0.185362)
 H01Y(0.178499) H01Q(0.480828) H01R(0.481074) H01S(0.489902) H01T(0.510106)
 H01U(0.52403) H01V(0.528349)
;
_shelx_res_checksum              76480
_shelx_hkl_checksum              67031
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.139
_oxdiff_exptl_absorpt_empirical_full_min 0.391