Pressure as a tool in crystal engineering: inducing a phase transition in a high-Z′ structure
Johnstone, Russell D. L.; Ieva, Maria; Lennie, Alistair R.; McNab, Hamish; Pidcock, Elna; Warren, John E.; Parsons, Simon; CrystEngComm 12 (2010) 2520–; doi:10.1039/b917290d

data_7211966
_publ_section_title
;
 Pressure as a tool in crystal engineering: inducing a phase transition in
 a high-Z&#x2032; structure
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              2520
_journal_paper_doi               10.1039/b917290d
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H15 N1 O2'
_chemical_formula_sum            'C20 H15 N O2'
_chemical_formula_weight         301.34
_chemical_name_common            'Methyl 2-(9H-carbazol-9-yl)benzoate'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 89.989(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   7.3592(7)
_cell_length_b                   14.601(2)
_cell_length_c                   51.188(9)
_cell_measurement_reflns_used    1559
_cell_measurement_temperature    293
_cell_measurement_theta_max      13
_cell_measurement_theta_min      2
_cell_volume                     5500.2(13)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         1500000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.782
_diffrn_measured_fraction_theta_max 0.733
_diffrn_measurement_device       APEX-II
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.47620
_diffrn_reflns_av_R_equivalents  0.1432
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17318
_diffrn_reflns_reduction_process
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;
_diffrn_reflns_theta_full        10.279
_diffrn_reflns_theta_max         13.705
_diffrn_reflns_theta_min         1.076
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_recrystallization_method
;
A mixture of carbazole, methyl 2-iodobenzoate,
copper powder, potassium carbonate and nitrobenzene
were heated at 175 degrees C for 48 h. After cooling,
the resultant mixture was a red solid.
A mixture of water/chloroform (1:1) was added to the solid,
and the two layers separated. The aqueous layer was
then extracted twice with chloroform, and the
organic layers were combined and dried over MgSO4.
The solvent was removed under reduced pressure,
and the residue oil was purified by flash dry chromatography
on silica using hexane/ethyl acetate (85:15) as the eluant.
This resulted in the formation of colourless crystals.
(5.30 g, 88%)
;
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         3239
_refine_ls_number_restraints     1154
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.028935
_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:
8.66 -4.45 4.72
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1309
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0899
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              43
_reflns_limit_l_min              0
_reflns_number_gt                3239
_reflns_number_total             4178
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            b917290d.txt
_cod_data_source_block           1_5GPa_I.cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5500.2(14)
_cod_original_sg_symbol_H-M      'P 1 n 1 '
_cod_original_formula_sum        'C20 H15 N1 O2'
_cod_database_code               7211966