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_7232897
_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                 95.935(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6132(7)
_cell_length_b                   14.5917(8)
_cell_length_c                   6.2617(3)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    224.0
_cell_measurement_theta_max      66.75
_cell_measurement_theta_min      4.45
_cell_volume                     1237.16(11)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_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      224.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_collimation    'focussed source'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            17860
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        66.741
_diffrn_reflns_theta_max         66.741
_diffrn_reflns_theta_min         3.264
_diffrn_source                   'Bruker TXS with Helios Optics'
_diffrn_source_type
;
'Incoatec microfocus 3.0 (Cu) X-ray Source'
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.1300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1733 before and 0.1013 after correction.
The Ratio of minimum to maximum transmission is 0.1727.
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    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             464
_exptl_crystal_preparation
;
Crystal grown inside capillary in-situ on
diffractmeter through cryogenic control
;
_exptl_crystal_recrystallization_method
'Grown from pure liquid at low temperature'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0929P)^2^+0.1289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1896
_reflns_number_total             2126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00870e2.cif
_cod_data_source_block           anisole_lt
_cod_depositor_comments
'Adding full bibliography for 7232896--7232897.cif.'
_cod_database_code               7232897
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.942
_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.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C8'(H8'), C4'(H4'), C4(H4), C7(H7), C5(H5), C6(H6), C7'(H7'),
 C5'(H5'), C6'(H6')
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1'(H1'A,H1'B,H1'C)
;
_olex2_exptl_crystal_mounting_method Capillary
_olex2_submission_special_instructions 'No special instructions were received'