Toward the synthesis of a highly strained hydrocarbon belt.
Shi, Tan-Hao; Guo, Qing-Hui; Tong, Shuo; Wang, Mei-Xiang; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00112

data_4134251
_publ_section_title
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 Toward the synthesis of a highly strained hydrocarbon belt.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00112
_journal_year                    2020
_chemical_formula_moiety         'C48 H56, 0.05(C1 H1 Cl3), 0.95(C H4 O)'
_chemical_formula_sum            'C49 H59.8 Cl0.2 O0.9'
_chemical_formula_weight         669.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                100.365(3)
_cell_angle_beta                 98.374(2)
_cell_angle_gamma                111.432(2)
_cell_formula_units_Z            2
_cell_length_a                   10.602(3)
_cell_length_b                   12.553(3)
_cell_length_c                   16.667(4)
_cell_measurement_reflns_used    6008
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4854
_cell_measurement_theta_min      1.8014
_cell_volume                     1976.2(9)
_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, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.4000
_diffrn_measured_fraction_theta_max 27.4854
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 13.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9183
	          2theta: -20.1175
scan:
	Number of images: 350
	           Slice: -110.0000 - 65.0000
	     Image width: 0.5000
	        Exp time: 13.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 44.9183
	          2theta: -20.1175
scan:
	Number of images: 346
	           Slice: -110.0000 - 63.0000
	     Image width: 0.5000
	        Exp time: 13.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9183
	          2theta: -20.1175
scan:
	Number of images: 224
	           Slice: -83.7500 - 28.2500
	     Image width: 0.5000
	        Exp time: 13.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9183
	          2theta: -20.1175
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0697
_diffrn_orient_matrix_UB_12      -0.0659
_diffrn_orient_matrix_UB_13      -0.0404
_diffrn_orient_matrix_UB_21      0.0181
_diffrn_orient_matrix_UB_22      -0.0851
_diffrn_orient_matrix_UB_23      0.0159
_diffrn_orient_matrix_UB_31      -0.0359
_diffrn_orient_matrix_UB_32      -0.0149
_diffrn_orient_matrix_UB_33      0.0491
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27701
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.801
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9007
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0633P)^2^+1.1255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8405
_reflns_number_total             9007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_003.cif
_cod_data_source_block           mx5444
_cod_original_cell_volume        1976.4(8)
_cod_database_code               4134251
_diffrn_number_total             9011
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 Cl2-C49 = Cl3-C49 = Cl1-C49
 1.76 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3 \\sim C49 \\sim O1 \\sim C50: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(O1) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(O1)=Sof(H1)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C49)=Sof(H49)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C22(H22), C36(H36), C46(H46), C49(H49)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C42(H42A,H42B), C47(H47A,H47B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C9(H9), C13(H13), C27(H27), C31(H31), C32(H32),
 C34(H34), C38(H38)
5.d X=CH2 refined with riding coordinates:
 C16(H16A,H16B), C40(H40A,H40B)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C24(H24A,H24B,H24C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              51578
_shelx_hkl_checksum              42450
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'