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_7211964
_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                 89.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   7.6168(2)
_cell_length_b                   15.2552(5)
_cell_length_c                   52.3376(16)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     6081.4(3)
_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_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39621
_diffrn_reflns_reduction_process
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;
_diffrn_reflns_theta_full        23.283
_diffrn_reflns_theta_max         23.283
_diffrn_reflns_theta_min         1.335
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_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          0.67
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.52
_refine_diff_density_max         0.13
_refine_diff_density_min         -0.14
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0526
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1658
_refine_ls_number_reflns         8633
_refine_ls_number_restraints     3082
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.008442
_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:
2.11 -1.90 1.23
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0242
_refine_ls_wR_factor_gt          0.0241
_refine_ls_wR_factor_ref         0.0241
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              58
_reflns_limit_l_min              0
_reflns_number_gt                8633
_reflns_number_total             8753
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            b917290d.txt
_cod_data_source_block           ambient_150K.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_sg_symbol_H-M      'P 1 n 1 '
_cod_original_formula_sum        'C20 H15 N1 O2'
_cod_database_code               7211964