A structural exploration of anisole accessed through extreme crystallisation conditions
Smith, Ellie Louvain; Ridout, Joe; Sellars, Jonathan David; Probert, Michael Richard; CrystEngComm 21 (2019) 4422–; doi:10.1039/C9CE00870E

data_7232896
_publ_section_title
;
 A structural exploration of anisole accessed through extreme
 crystallisation conditions
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              4422
_journal_paper_doi               10.1039/C9CE00870E
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C7 H8 O'
_chemical_formula_sum            'C7 H8 O'
_chemical_formula_weight         108.13
_chemical_name_systematic        methoxybenzene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-24
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-25 deposited with the CCDC.    2019-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.401(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.700(4)
_cell_length_b                   5.4468(8)
_cell_length_c                   7.8567(11)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      17.53
_cell_measurement_theta_min      3.60
_cell_volume                     580.0(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.392
_diffrn_measured_fraction_theta_max 0.392
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.392
_diffrn_reflns_Laue_measured_fraction_max 0.392
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2664
_diffrn_reflns_point_group_measured_fraction_full 0.392
_diffrn_reflns_point_group_measured_fraction_max 0.392
_diffrn_reflns_theta_full        18.131
_diffrn_reflns_theta_max         18.131
_diffrn_reflns_theta_min         3.605
_diffrn_source                   'Bruker TXS with Helios Optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.6293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0605 before and 0.0385 after correction.
The Ratio of minimum to maximum transmission is 0.8456.
The \l/2 correction factor is Not present.
;
_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    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_preparation
'Crystal grown inside diamond anvil cell at high pressure'
_exptl_crystal_recrystallization_method
'Crystal grown inside diamond anvil cell at high pressure'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.094
_refine_diff_density_min         -0.088
_refine_diff_density_rms         0.025
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         326
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0223P)^2^+0.4505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                231
_reflns_number_total             326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00870e2.cif
_cod_data_source_block           anisole_new
_cod_depositor_comments
'Adding full bibliography for 7232896--7232897.cif.'
_cod_database_code               7232896
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C6(H6), C4(H4), C7(H7)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_exptl_crystal_mounting_method
;
Crystal mounted onto diffractometer using
custom grip for diamond anvil cell into standard
goniometer head
;
_olex2_submission_special_instructions 'No special instructions were received'