#------------------------------------------------------------------------------
#$Date: 2019-07-25 02:22:42 +0200 (jue 25 de jul de 2019) $
#$Revision: 217249 $
#$URL: svn://www.crystallography.net/cod/cif/1/55/21/1552131.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1552131
loop_
_publ_author_name
'Li, Liang'
'Commins, Patrick'
'Al-Handawi, Marieh B.'
'Karothu, Durga Prasad'
'Halabi, Jad Mahmoud'
'Schramm, Stefan'
'Weston, James'
'Rezgui, Rachid'
'Naumov, Panče'
_publ_section_title
;
 Martensitic organic crystals as soft actuators
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02444A
_journal_year                    2019
_chemical_formula_moiety         'C12 H18'
_chemical_formula_sum            'C12 H18'
_chemical_formula_weight         162.26
_chemical_name_systematic        HMB
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2304ny
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-26 deposited with the CCDC.    2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                104.05(2)
_cell_angle_beta                 99.08(2)
_cell_angle_gamma                99.34(2)
_cell_formula_units_Z            1
_cell_length_a                   5.322(8)
_cell_length_b                   6.293(10)
_cell_length_c                   8.099(12)
_cell_measurement_reflns_used    2050
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.65
_cell_volume                     254.1(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3101
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.988
_diffrn_reflns_theta_min         2.649
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       plate
_exptl_crystal_F_000             90
_exptl_crystal_size_max          1.465
_exptl_crystal_size_mid          0.461
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0675
_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/[σ²(Fo²)+(0.1335P)²+0.0602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2211
_refine_ls_wR_factor_ref         0.2318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                833
_reflns_number_total             990
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
    mo_hmb0424_0m.res created by SHELXL-2014/7

TITL mo_HMB0424_0m in P-1 #2
REM Best SHELXD solution FINAL CC 86.91
REM Fragments: 6
REM reset to P-1 #2
CELL 0.71073 5.3221 6.2935 8.0989 104.0473 99.0843 99.3369
ZERR 1 0.0082 0.0097 0.0124 0.0204 0.0208 0.0208
LATT 1
SFAC C H
UNIT 12 18
 
L.S. 14
PLAN  5
SIZE 0.148 0.461 1.465
TEMP 23
CONF
fmap 2
acta
OMIT 0 52
REM <olex2.extras>
REM <HklSrc "%.\\mo_HMB0424_0m.hkl">
REM </olex2.extras>
 
WGHT    0.133500    0.060200
FVAR       0.54298
C5    1    0.819688    0.569208    0.389169    11.00000    0.03573    0.04202 =
         0.04878    0.01923    0.00469    0.00701
C6    1    0.931267    0.387311    0.322068    11.00000    0.04074    0.04275 =
         0.04060    0.01169    0.00712    0.00494
C4    1    0.887924    0.680732    0.567257    11.00000    0.03843    0.03554 =
         0.05180    0.01340    0.01170    0.00859
C12   1    0.626419    0.645330    0.270574    11.00000    0.05648    0.07157 =
         0.07068    0.02994   -0.00088    0.02253
AFIX 137
H12A  2    0.655574    0.603608    0.154132    11.00000   -1.50000
H12B  2    0.647993    0.805135    0.309894    11.00000   -1.50000
H12C  2    0.452849    0.575629    0.272320    11.00000   -1.50000
AFIX   0
C11   1    0.762418    0.874098    0.638309    11.00000    0.06190    0.05020 =
         0.07753    0.01178    0.01950    0.02315
AFIX 137
H11A  2    0.827822    1.000266    0.598938    11.00000   -1.50000
H11B  2    0.802871    0.914547    0.763125    11.00000   -1.50000
H11C  2    0.577174    0.829790    0.597804    11.00000   -1.50000
AFIX   0
C10   1    0.855833    0.264953    0.130123    11.00000    0.07998    0.07049 =
         0.04638    0.00802    0.00691    0.01802
AFIX 137
H10A  2    0.709267    0.313498    0.077077    11.00000   -1.50000
H10B  2    0.810627    0.106633    0.115867    11.00000   -1.50000
H10C  2    0.999772    0.297142    0.075718    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM  mo_HMB0424_0m in P-1 #2
REM R1 =  0.0675 for     833 Fo > 4sig(Fo)  and  0.0753 for all     990 data
REM     58 parameters refined using      0 restraints
 
END  
     
WGHT      0.1336      0.0603 

REM Highest difference peak  0.304,  deepest hole -0.180,  1-sigma level  0.052
Q1    1   0.8709  0.4767  0.3558  11.00000  0.05    0.30
Q2    1   1.0471  0.3750  0.3722  11.00000  0.05    0.25
Q3    1   0.4848  0.7068  0.3414  11.00000  0.05    0.22
Q4    1   0.5180  0.5018  0.1780  11.00000  0.05    0.22
Q5    1   0.8083  0.5789  0.4571  11.00000  0.05    0.20

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0675 for 833 Fo > 4sig(Fo) and 0.0753 for all 3655 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.30, deepest hole -0.18
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0753
  REM R1_gt = 0.0675
  REM wR_ref = 0.2318
  REM GOOF = 1.123
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3655
  REM Reflections_gt = 833
  REM Parameters = n/a
  REM Hole = -0.18
  REM Peak = 0.30
  REM Flack = n/a
;
_cod_data_source_file            c9sc02444a11.cif
_cod_data_source_block           mo_hmb0424_0m
_cod_database_code               1552131
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C11(H11a,H11b,H11c), C10(H10a,H10b,H10c)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
C5 C 0.8197(3) 0.5692(3) 0.3892(2) 0.0416(6) Uani 1 1 d .
C6 C 0.9313(3) 0.3873(3) 0.3221(2) 0.0419(6) Uani 1 1 d .
C4 C 0.8879(3) 0.6807(3) 0.5673(2) 0.0413(6) Uani 1 1 d .
C12 C 0.6264(4) 0.6453(4) 0.2706(3) 0.0649(7) Uani 1 1 d .
H12A H 0.6556 0.6036 0.1541 0.097 Uiso 1 1 calc GR
H12B H 0.6480 0.8051 0.3099 0.097 Uiso 1 1 calc GR
H12C H 0.4528 0.5756 0.2723 0.097 Uiso 1 1 calc GR
C11 C 0.7624(4) 0.8741(4) 0.6383(3) 0.0623(7) Uani 1 1 d .
H11A H 0.8278 1.0003 0.5989 0.093 Uiso 1 1 calc GR
H11B H 0.8029 0.9145 0.7631 0.093 Uiso 1 1 calc GR
H11C H 0.5772 0.8298 0.5978 0.093 Uiso 1 1 calc GR
C10 C 0.8558(5) 0.2650(4) 0.1301(3) 0.0675(7) Uani 1 1 d .
H10A H 0.7093 0.3135 0.0771 0.101 Uiso 1 1 calc GR
H10B H 0.8106 0.1066 0.1159 0.101 Uiso 1 1 calc GR
H10C H 0.9998 0.2971 0.0757 0.101 Uiso 1 1 calc GR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C5 0.0357(9) 0.0420(10) 0.0488(11) 0.0192(8) 0.0047(7) 0.0070(7)
C6 0.0407(10) 0.0428(10) 0.0406(10) 0.0117(7) 0.0071(7) 0.0049(7)
C4 0.0384(9) 0.0355(9) 0.0518(11) 0.0134(7) 0.0117(7) 0.0086(7)
C12 0.0565(12) 0.0716(14) 0.0707(15) 0.0299(12) -0.0009(10) 0.0225(10)
C11 0.0619(13) 0.0502(12) 0.0775(16) 0.0118(10) 0.0195(11) 0.0232(10)
C10 0.0800(16) 0.0705(15) 0.0464(13) 0.0080(10) 0.0069(10) 0.0180(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
C6 C5 C12 120.4(2) .
C4 C5 C6 119.88(18) .
C4 C5 C12 119.7(2) .
C5 C6 C10 120.01(19) .
C4 C6 C5 120.03(19) 2_766
C4 C6 C10 120.0(2) 2_766
C5 C4 C11 119.29(18) .
C6 C4 C5 120.09(19) 2_766
C6 C4 C11 120.6(2) 2_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C5 C6 1.407(3) .
C5 C4 1.402(3) .
C5 C12 1.510(3) .
C6 C4 1.400(3) 2_766
C6 C10 1.514(3) .
C4 C6 1.400(3) 2_766
C4 C11 1.518(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C6 C5 C4 C6 0.6(3) 2_766
C6 C5 C4 C11 -178.94(14) .
C4 C5 C6 C4 -0.6(3) 2_766
C4 C5 C6 C10 179.35(15) .
C12 C5 C6 C4 179.41(14) 2_766
C12 C5 C6 C10 -0.6(3) .
C12 C5 C4 C6 -179.41(14) 2_766
C12 C5 C4 C11 1.0(3) .
