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

data_7228064
_publ_section_title
;
 Mixed halide/oxoanion-templated frameworks
;
_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, 4(N O3), 1.5(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C30.5 H39 N12 O14'
_chemical_formula_weight         1595.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2017-02-06 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                101.982(7)
_cell_angle_beta                 91.167(8)
_cell_angle_gamma                90.664(8)
_cell_formula_units_Z            4
_cell_length_a                   11.6729(15)
_cell_length_b                   11.8954(9)
_cell_length_c                   26.963(2)
_cell_measurement_reflns_used    4419
_cell_measurement_temperature    150
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      3.85
_cell_volume                     3661.1(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.041
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22057
_diffrn_reflns_theta_full        68.252
_diffrn_reflns_theta_max         68.252
_diffrn_reflns_theta_min         3.788
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1671.990
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9703
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         11000
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.1386
_refine_ls_shift/su_max          0.0001955
_refine_ls_shift/su_mean         0.0000140
_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: 
 0.341E+04 0.560E+04 0.338E+04 0.137E+04 325. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3474
_refine_ls_wR_factor_gt          0.3309
_refine_ls_wR_factor_ref         0.3474
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                7779
_reflns_number_total             12917
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.74
_oxford_diffrn_Wilson_scale      0.14
_oxford_refine_ls_r_factor_ref   0.1618
_oxford_refine_ls_scale          3.54(9)
_oxford_reflns_number_all        11000
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7ce00265c2.cif
_cod_data_source_block           1NO3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7228063--7228067.cif.

2017-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C61 H78 N24 O28'
_cod_original_formula_weight         1595.44
_cod_original_formula_moiety         '2(C29 H32 N8), 8(N O3), 3(C H4 O), H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3661.1(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7228064
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S  U'S 
SUMFIX ELEMENT SCALES 
RIDE N   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE N   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
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) 
RIDE N   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE N   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE N   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE N   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE N   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE N   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE N   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE N   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE N   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) 
RIDE N   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE N   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE N   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE N   (  81,X'S) H   ( 811,X'S) H   ( 812,X'S) 
RIDE N   (  82,X'S) H   ( 821,X'S) H   ( 822,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
RIDE O   ( 201,X'S) H   (2011,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) H   (2022,X'S) H   (2023,X'S) 
RIDE O   ( 211,X'S) H   (2111,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) H   (2122,X'S) H   (2123,X'S) 
RIDE O   ( 221,X'S) H   (2211,X'S) 
RIDE C   ( 222,X'S) H   (2221,X'S) H   (2222,X'S) H   (2223,X'S) 
RIDE O   ( 231,X'S) H   (2311,X'S) H   (2312,X'S) 
END 
;
_iucr_refine_instructions_details_restraints
;                                                                       
REM 
REM MEOHS 
REM 
DIST 1.45, 0.01 = O(201) TO C(202), O(211) TO C(212) 
CONT O(221) TO C(222) 
REM 
REM NITRATES REM 
DIST 0, 0.01 = MEAN N(101) TO O(102), N(101) TO O(103) 
CONT N(101) TO O(104) 
CONT N(111) TO O(112), N(111) TO O(113) 
CONT N(111) TO O(114) 
CONT N(121) TO O(122), N(121) TO O(123) 
CONT N(121) TO O(124) 
CONT N(131) TO O(132), N(131) TO O(133) 
CONT N(131) TO O(134) 
CONT N(141) TO O(142), N(141) TO O(143) 
CONT N(141) TO O(144) 
CONT N(151) TO O(152), N(151) TO O(153) 
CONT N(151) TO O(154) 
CONT N(161) TO O(162), N(161) TO O(163) 
CONT N(161) TO O(164) 
CONT N(171) TO O(172), N(171) TO O(173) 
CONT N(171) TO O(174) 
PLANAR N(141) O(142) O(143) O(144) 
PLANAR N(161) O(162) O(163) O(164) 
ANGL 120, 1 = O(142) TO N(141) TO O(143) 
CONT O(142) TO N(141) TO O(144) 
CONT O(143) TO N(141) TO O(144) 
CONT O(162) TO N(161) TO O(163) 
CONT O(162) TO N(161) TO O(164) 
CONT O(163) TO N(161) TO O(164) 
REM 
REM PHENYLS 
REM 
DIST 0, 0.01 = MEAN C(4) TO C(5), C(5) TO C(6) 
CONT C(6) TO C(7), C(7) TO C(8) 
CONT C(8) TO C(9), C(9) TO C(4) 
CONT C(14) TO C(15), C(15) TO C(16) 
CONT C(16) TO C(17), C(17) TO C(18) 
CONT C(18) TO C(19), C(19) TO C(14) 
CONT C(24) TO C(25), C(25) TO C(26) 
CONT C(26) TO C(27), C(27) TO C(28) 
CONT C(28) TO C(29), C(29) TO C(24) 
CONT C(34) TO C(35), C(35) TO C(36) 
CONT C(36) TO C(37), C(37) TO C(38) 
CONT C(38) TO C(39), C(39) TO C(34) 
CONT C(54) TO C(55), C(55) TO C(56) 
CONT C(56) TO C(57), C(57) TO C(58) 
CONT C(58) TO C(59), C(59) TO C(54) 
CONT C(64) TO C(65), C(65) TO C(66) 
CONT C(66) TO C(67), C(67) TO C(68) 
CONT C(68) TO C(69), C(69) TO C(64) 
CONT C(74) TO C(75), C(75) TO C(76) 
CONT C(76) TO C(77), C(77) TO C(78) 
CONT C(78) TO C(79), C(79) TO C(74) 
CONT C(84) TO C(85), C(85) TO C(86) 
CONT C(86) TO C(87), C(87) TO C(88) 
CONT C(88) TO C(89), C(89) TO C(84) 
REM 
REM OTHER 
REM 
DIST 0, 0.01 = MEAN N(1) TO C(3), N(2) TO C(3) 
CONT N(11) TO C(13), N(12) TO C(13) 
CONT N(21) TO C(23), N(22) TO C(23) 
CONT N(31) TO C(33), N(32) TO C(33) 
CONT N(51) TO C(53), N(52) TO C(53) 
CONT N(61) TO C(63), N(62) TO C(63) 
CONT N(71) TO C(73), N(72) TO C(73) 
CONT N(81) TO C(83), N(82) TO C(83) 
DIST 0, 0.01 = MEAN C(3) TO C(4), C(13) TO C(14) 
CONT C(23) TO C(24), C(33) TO C(34) 
CONT C(53) TO C(54), C(63) TO C(64) 
CONT C(73) TO C(74), C(83) TO C(84) 
DIST 0, 0.01 = MEAN C(7) TO C(10), C(17) TO C(10) 
CONT C(27) TO C(10), C(37) TO C(10) 
CONT C(57) TO C(60), C(67) TO C(60) 
CONT C(77) TO C(60), C(87) TO C(60) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00100 = N(141) TO O(142) 
VIBR .0, 0.00100 = N(141) TO O(143) 
VIBR .0, 0.00100 = N(141) TO O(144) 
VIBR .0, 0.00200 = O(143) TO O(142) 
VIBR .0, 0.00200 = O(144) TO O(142) 
VIBR .0, 0.00200 = O(144) TO O(143) 
VIBR .0, 0.00100 = N(161) TO O(162) 
VIBR .0, 0.00100 = N(161) TO O(163) 
VIBR .0, 0.00100 = N(161) TO O(164) 
VIBR .0, 0.00200 = O(163) TO O(162) 
VIBR .0, 0.00200 = O(164) TO O(162) 
VIBR .0, 0.00200 = O(164) TO O(163) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.01000 = N(141) TO O(142) 
U(IJ) .0, 0.01000 = N(141) TO O(143) 
U(IJ) .0, 0.01000 = N(141) TO O(144) 
U(IJ) .0, 0.01000 = N(161) TO O(162) 
U(IJ) .0, 0.01000 = N(161) TO O(163) 
U(IJ) .0, 0.01000 = N(161) TO O(164) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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