Colossal thermal expansion and negative thermal expansion in simple halogen bonded complexes
Jones, Richard H.; Knight, Kevin S.; Marshall, William G.; Clews, John; Darton, Richard J.; Pyatt, Daniel; Coles, Simon J.; Horton, Peter N.; CrystEngComm 16 (2014) 237–; doi:10.1039/c3ce41909f

data_7213568
_publ_section_title
;
 Colossal thermal expansion and negative thermal expansion in simple
 halogen bonded complexes
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              237
_journal_paper_doi               10.1039/c3ce41909f
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C5 H5 Br1 I1 N1'
_chemical_formula_sum            'C5 H5 Br I N'
_chemical_formula_weight         285.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 97.706(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.3813(2)
_cell_length_b                   12.6339(5)
_cell_length_c                   14.1942(4)
_cell_measurement_reflns_used    10231
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     778.59(5)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8997
_diffrn_reflns_theta_full        27.544
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         3.225
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.150
_exptl_absorpt_correction_T_max  0.09
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.59
_refine_diff_density_min         -1.16
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0417
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1606
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.0145432
_refine_ls_shift/su_mean         0.0010232
_refine_ls_structure_factor_coef Fsqd
_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: 
 49.5 76.6 40.8 11.6 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1079
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1079
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1337
_reflns_number_total             1793
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.39
_oxford_diffrn_Wilson_scale      3.57
_oxford_refine_ls_r_factor_ref   0.0455
_oxford_refine_ls_scale          0.5582(16)
_oxford_reflns_number_all        1606
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3ce41909f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C5 H5 Br1 I1 N1'
_cod_database_code               7213568
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT I    (    1 ,X'S,U'S)  UNTIL C    (    6 ) 
CONT H    (    2 ,X'S,U[ISO])  UNTIL H    (    6 ) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 2) TO H(2) 
REST 0.080, 0.002 = H(2,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(2) TO C ( 2) TO N(1) 
CONT H(2) TO C ( 2) TO C(3) 
PLANAR C ( 2) N(1) C(3) H(2) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 3) TO H(3) 
REST 0.100, 0.002 = H(3,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(3) TO C ( 3) TO C(2) 
CONT H(3) TO C ( 3) TO C(4) 
PLANAR C ( 3) C(2) C(4) H(3) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 4) TO H(4) 
REST 0.100, 0.002 = H(4,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(4) TO C ( 4) TO C(3) 
CONT H(4) TO C ( 4) TO C(5) 
PLANAR C ( 4) C(3) C(5) H(4) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 5) TO H(5) 
REST 0.098, 0.002 = H(5,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(5) TO C ( 5) TO C(4) 
CONT H(5) TO C ( 5) TO C(6) 
PLANAR C ( 5) C(4) C(6) H(5) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 6) TO H(6) 
REST 0.080, 0.002 = H(6,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(6) TO C ( 6) TO C(5) 
CONT H(6) TO C ( 6) TO N(1) 
PLANAR C ( 6) C(5) N(1) H(6) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;