Mixed halide/oxoanion-templated frameworks
Morshedi, Mahbod; White, Nicholas G.; CrystEngComm 19 (2017) 2367–; doi:10.1039/C7CE00265C

data_7228065
_publ_section_title
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 Mixed halide/oxoanion-templated frameworks
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_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2367
_journal_paper_doi               10.1039/C7CE00265C
_journal_volume                  19
_journal_year                    2017
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C29 H32 N8, 2(Br), C2 O4'
_chemical_formula_sum            'C31 H32 Br2 N8 O4'
_chemical_formula_weight         740.45
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
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2017-02-06 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.07173(18)
_cell_length_b                   12.07173(18)
_cell_length_c                   11.3545(3)
_cell_measurement_reflns_used    7794
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.5
_cell_measurement_theta_min      3.89
_cell_volume                     1654.65(6)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15992
_diffrn_reflns_theta_full        72.289
_diffrn_reflns_theta_max         73.764
_diffrn_reflns_theta_min         3.893
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.506
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
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_refine_diff_density_max         2.36
_refine_diff_density_min         -1.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1665
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.0001049
_refine_ls_shift/su_mean         0.0000106
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
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 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: 
 0.449E+04 0.729E+04 0.477E+04 0.236E+04 571. 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1880
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.1880
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1591
_reflns_number_total             1673
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.55
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0754
_oxford_refine_ls_scale          4.56(19)
_oxford_reflns_number_all        1665
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7ce00265c2.cif
_cod_data_source_block           1OxBr
_cod_depositor_comments
'Adding full bibliography for 7228063--7228067.cif.'
_cod_original_cell_volume        1654.66(4)
_cod_original_sg_symbol_H-M      'P 4/n '
_cod_database_code               7228065
_iucr_refine_instructions_details_constraints
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BLOCK 
CONT SCALE 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   12 ) 
CONT H    (   22 ,X'S)  UNTIL H    (   11 ) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
END  
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_iucr_refine_instructions_details_restraints
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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            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 1) TO H(12) 
CONT N ( 1) TO H(11) 
REST 0.031, 0.002 = H(12,U[ISO]) 
REST 0.031, 0.002 = H(11,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(3) TO N ( 1) TO H(12) 
CONT C(3) TO N ( 1) TO H(11) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 2) TO H(22) 
CONT N ( 2) TO H(21) 
REST 0.037, 0.002 = H(22,U[ISO]) 
REST 0.037, 0.002 = H(21,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(3) TO N ( 2) TO H(22) 
CONT C(3) TO N ( 2) TO H(21) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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