Crystal structures of eight mono-methyl alkanes (C~26~–C~32~) <i>via</i> single-crystal and powder diffraction and DFT-D optimization
Brooks, Lee; Brunelli, Michela; Pattison, Philip; Jones, Graeme R.; Fitch, Andrew; IUCrJ 2 (2015) 490–497; doi:10.1107/S2052252515010271

data_1542826
_publ_section_title
;
 Crystal structures of eight mono-methyl alkanes (C~26~--C~32~) <i>via</i>
 single-crystal and powder diffraction and DFT-D optimization
;
_journal_coeditor_code           LC5062SUP1
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_page_first              490
_journal_page_last               497
_journal_paper_doi               10.1107/S2052252515010271
_journal_volume                  2
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_compound_source        'Synthesized by Lee Brooks, Keele University'
_chemical_formula_moiety         'C30 H62'
_chemical_formula_sum            'C30 H62'
_chemical_formula_weight         422.81
_chemical_name_systematic
;
(<i>S</i>)-7-methylnonacosane
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             13-10-15
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2015-07-05 # Formatted by IUCr publCIF system
;
_cell_angle_alpha                90
_cell_angle_beta                 90.30(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.172(5)
_cell_length_b                   4.935(1)
_cell_length_c                   10.375(2)
_cell_measurement_temperature    120
_cell_volume                     1442.4(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'CrysAlis, Oxford Diffraction'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'MAR 345 image plate'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.82
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7987
_diffrn_reflns_theta_full        23.821
_diffrn_reflns_theta_max         24.308
_diffrn_reflns_theta_min         1.668
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1657
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.0005425
_refine_ls_shift/su_mean         0.0000709
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 11.7 3.20 5.94 2.87 0.607 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0804
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0804
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              4
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1662
_reflns_number_total             1679
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   -2.02
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0851
_oxford_refine_ls_scale          10.07(5)
_oxford_reflns_number_all        1665
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_publcif_datablock.id            {bf95e2e8-93dd-4f9f-a1f8-a55e39106173}
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U[ISO] 
RIDE C  (  1,X'S) H  ( 11,X'S) H  ( 12,X'S) H  ( 13,X'S) 
RIDE C  (  2,X'S) H  ( 21,X'S) H  ( 22,X'S) 
RIDE C  (  3,X'S) H  ( 31,X'S) H  ( 32,X'S) 
RIDE C  (  4,X'S) H  ( 41,X'S) H  ( 42,X'S) 
RIDE C  (  5,X'S) H  ( 51,X'S) H  ( 52,X'S) 
RIDE C  (  6,X'S) H  ( 61,X'S) H  ( 62,X'S) 
RIDE C  (  7,X'S) H  ( 71,X'S) 
RIDE C  (  8,X'S) H  ( 81,X'S) H  ( 82,X'S) 
RIDE C  (  9,X'S) H  ( 91,X'S) H  ( 92,X'S) 
RIDE C  ( 10,X'S) H  ( 101,X'S) H  ( 102,X'S) 
RIDE C  ( 11,X'S) H  ( 111,X'S) H  ( 112,X'S) 
RIDE C  ( 12,X'S) H  ( 121,X'S) H  ( 122,X'S) 
RIDE C  ( 13,X'S) H  ( 131,X'S) H  ( 132,X'S) 
RIDE C  ( 14,X'S) H  ( 141,X'S) H  ( 142,X'S) 
RIDE C  ( 15,X'S) H  ( 151,X'S) H  ( 152,X'S) 
RIDE C  ( 16,X'S) H  ( 161,X'S) H  ( 162,X'S) 
RIDE C  ( 17,X'S) H  ( 171,X'S) H  ( 172,X'S) 
RIDE C  ( 18,X'S) H  ( 181,X'S) H  ( 182,X'S) 
RIDE C  ( 19,X'S) H  ( 191,X'S) H  ( 192,X'S) 
RIDE C  ( 20,X'S) H  ( 201,X'S) H  ( 202,X'S) 
RIDE C  ( 21,X'S) H  ( 211,X'S) H  ( 212,X'S) 
RIDE C  ( 22,X'S) H  ( 221,X'S) H  ( 222,X'S) 
RIDE C  ( 23,X'S) H  ( 231,X'S) H  ( 232,X'S) 
RIDE C  ( 24,X'S) H  ( 241,X'S) H  ( 242,X'S) 
RIDE C  ( 25,X'S) H  ( 251,X'S) H  ( 252,X'S) 
RIDE C  ( 26,X'S) H  ( 261,X'S) H  ( 262,X'S) 
RIDE C  ( 27,X'S) H  ( 271,X'S) H  ( 272,X'S) 
RIDE C  ( 28,X'S) H  ( 281,X'S) H  ( 282,X'S) 
RIDE C  ( 29,X'S) H  ( 291,X'S) H  ( 292,X'S) H  ( 293,X'S) 
RIDE C  ( 30,X'S) H  ( 301,X'S) H  ( 302,X'S) H  ( 303,X'S) 
END                                       
;
_iucr_refine_instructions_details_restraints
;
NO 
REM  HREST  START (DO NOT REMOVE THIS LINE) 
REM  HREST  END (DO NOT REMOVE THIS LINE) 
END                                       
;
_cod_data_source_file            lc5062.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               1542826