Syntheses, Crystal Structures, and Properties of Two 2-Fold Interpenetrating Metal‒Organic Frameworks Based on a Trigonal Rigid Ligand
Yang, Jie; Wang, Xiaoqing; Wang, Rongming; Zhang, Liangliang; Liu, Fuling; Dai, Fangna; Sun, Daofeng; Crystal Growth & Design 14 (2014) 6521–; doi:10.1021/cg501425x

data_4512334
_publ_section_title
;
 Syntheses, Crystal Structures, and Properties of Two 2-Fold
 Interpenetrating Metal--Organic Frameworks Based on a Trigonal Rigid
 Ligand
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6521
_journal_paper_doi               10.1021/cg501425x
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         '2(C83.5 H72 Mn3 N3.5 O17)'
_chemical_formula_sum            'C167 H144 Mn6 N7 O34'
_chemical_formula_weight         3122.53
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                62.572(3)
_cell_angle_beta                 82.489(3)
_cell_angle_gamma                73.850(3)
_cell_formula_units_Z            1
_cell_length_a                   13.8783(5)
_cell_length_b                   20.3674(8)
_cell_length_c                   21.0344(5)
_cell_measurement_reflns_used    8130
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.8320
_cell_measurement_theta_min      3.6660
_cell_volume                     5069.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.0450
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   41.00   67.00   1.0000    4.1800
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 26

  2 omega  -21.00   67.00   1.0000    4.1800
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 88

  3 omega  -67.00   22.00   1.0000    4.1800
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 89

  4 omega   46.00  107.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   19.0000  -90.0000 61

  5 omega   50.00   75.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  120.0000 25

  6 omega   -6.00   47.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  150.0000 53

  7 omega   32.00  116.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   90.0000 84

  8 omega    5.00   61.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -30.0000 56

  9 omega   28.00  118.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 90

 10 omega   69.00  121.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 52

 11 omega   32.00  110.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  -90.0000 78

 12 omega   38.00  104.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -120.0000 66

 13 omega  101.00  147.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 46

 14 omega   40.00   93.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -30.0000 53

 15 omega   40.00   79.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 39

 16 omega  100.00  178.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 78

 17 omega   65.00  129.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000 -180.0000 64

 18 omega   35.00   71.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -120.0000 36

 19 omega   41.00   93.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 52

 20 omega   84.00  111.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

 21 omega   90.00  173.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -120.0000 83

 22 omega   45.00  120.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  150.0000 75

 23 omega   55.00  112.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 57

 24 omega   34.00   91.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 57

 25 omega   50.00   92.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 42

 26 omega   38.00  110.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 72

 27 omega   88.00  115.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 27

 28 omega   79.00  106.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 27

 29 omega   34.00   93.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 59

 30 omega   67.00  147.00   1.0000   16.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000 -120.0000 80

 31 omega  -32.00   71.00   1.0000    4.1800
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0972386000
_diffrn_orient_matrix_UB_12      -0.0035534000
_diffrn_orient_matrix_UB_13      -0.0442884000
_diffrn_orient_matrix_UB_21      -0.0041872000
_diffrn_orient_matrix_UB_22      0.0828621000
_diffrn_orient_matrix_UB_23      -0.0170631000
_diffrn_orient_matrix_UB_31      0.0623122000
_diffrn_orient_matrix_UB_32      -0.0292896000
_diffrn_orient_matrix_UB_33      0.0674999000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37565
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       virgate
_exptl_crystal_F_000             1617
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         18916
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.1156
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3552
_refine_ls_wR_factor_ref         0.3883
_reflns_number_gt                11491
_reflns_number_total             18916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501425x_si_002.cif
_cod_data_source_block           yj-1441
_cod_depositor_comments
'Adding full bibliography for 4512334--4512335.cif.'
_cod_database_code               4512334
_chemical_oxdiff_formula         'C H O Mn'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: N1(0.5) C82(0.5)
 Fixed Uiso: H1WA(0.114) H1WB(0.114) H2(0.125) H3(0.152) H5(0.146) H6(0.135)
 H15A(0.086) H15B(0.086) H15C(0.086) H17A(0.084) H17B(0.084) H17C(0.084)
 H18A(0.088) H18B(0.088) H18C(0.088) H22(0.077) H23(0.074) H25(0.082)
 H26(0.081) H31(0.077) H32(0.077) H34(0.073) H35(0.071) H39(0.089) H40(0.095)
 H42(0.075) H43(0.08) H52A(0.08) H52B(0.08) H52C(0.08) H53A(0.086) H53B(0.086)
 H53C(0.086) H55A(0.087) H55B(0.087) H55C(0.087) H59(0.078) H60(0.071)
 H62(0.07) H63(0.07) H67(0.091) H68(0.088) H70(0.068) H71(0.071) H73A(0.218)
 H73B(0.218) H73C(0.218) H74A(0.227) H74B(0.227) H74C(0.227) H75(0.123)
 H76A(0.224) H76B(0.224) H76C(0.224) H77A(0.352) H77B(0.352) H77C(0.352)
 H78(0.115) H81A(0.585) H81B(0.585) H81C(0.585) H82A(0.168) H82B(0.168)
 H82C(0.168) H83(0.124) H84A(0.31) H84B(0.31) H84C(0.31) H85A(0.343)
 H85B(0.343) H85C(0.343) H86(0.178)
 Fixed X: H1WA(0.4243) H1WB(0.5011) H2(0.7893) H3(0.7853) H5(0.5545)
 H6(0.5589) H15A(0.6309) H15B(0.5464) H15C(0.5235) H17A(0.6638) H17B(0.7697)
 H17C(0.7408) H18A(0.545) H18B(0.6511) H18C(0.6409) H22(0.901) H23(0.9608)
 H25(0.6913) H26(0.6292) H31(0.5722) H32(0.4841) H34(0.2371) H35(0.3254)
 H39(0.0972) H40(0.0987) H42(0.3181) H43(0.3162) H52A(0.0778) H52B(0.0971)
 H52C(0.1878) H53A(0.1793) H53B(0.2841) H53C(0.204) H55A(0.068) H55B(0.0083)
 H55C(0.1206) H59(0.0425) H60(0.0329) H62(0.1872) H63(0.2014) H67(-0.0851) H68(-
 0.1243) H70(0.0575) H71(0.0947) H73A(0.9341) H73B(0.9814) H73C(0.8775)
 H74A(0.7912) H74B(0.76) H74C(0.859) H75(0.8534) H76A(0.8147) H76B(0.907)
 H76C(0.8872) H77A(0.7452) H77B(0.7004) H77C(0.6609) H78(0.7684) H81A(0.4096)
 H81B(0.4954) H81C(0.4491) H82A(0.254) H82B(0.2499) H82C(0.3304) H83(0.3903)
 H84A(0.3254) H84B(0.3918) H84C(0.3168) H85A(0.5539) H85B(0.4638) H85C(0.482)
 H86(0.4884)
 Fixed Y: H1WA(0.2757) H1WB(0.302) H2(0.12) H3(0.0277) H5(0.1933) H6(0.27)
 H15A(0.1428) H15B(0.1464) H15C(0.1384) H17A(-0.1578) H17B(-0.1794) H17C(-
 0.1084) H18A(-0.0994) H18B(-0.0902) H18C(-0.1648) H22(-0.3457) H23(-0.4721)
 H25(-0.5099) H26(-0.3825) H31(0.1491) H32(0.2064) H34(0.1514) H35(0.0973)
 H39(0.5415) H40(0.6649) H42(0.6499) H43(0.5245) H52A(0.8661) H52B(0.9349)
 H52C(0.8689) H53A(0.8535) H53B(0.8704) H53C(0.9264) H55A(1.1652) H55B(1.1612)
 H55C(1.1657) H59(1.0655) H60(1.123) H62(1.2678) H63(1.208) H67(1.0777)
 H68(1.1417) H70(1.2751) H71(1.2143) H73A(-1.0113) H73B(-1.074) H73C(-1.0733)
 H74A(-0.996) H74B(-1.0428) H74C(-1.0766) H75(-0.9076) H76A(-0.7329) H76B(-
 0.6994) H76C(-0.7665) H77A(-0.5594) H77B(-0.6184) H77C(-0.5921) H78(-0.6364)
 H81A(0.4767) H81B(0.4098) H81C(0.4028) H82A(0.338) H82B(0.4126) H82C(0.3372)
 H83(0.3996) H84A(0.0422) H84B(-0.0196) H84C(0.0519) H85A(0.0384) H85B(0.0196)
 H85C(0.1017) H86(0.1526)
 Fixed Z: H1WA(0.407) H1WB(0.3633) H2(-0.4046) H3(-0.2736) H5(-0.2588) H6(-
 0.3793) H15A(-0.0678) H15B(-0.0113) H15C(-0.0781) H17A(-0.0379) H17B(-0.005)
 H17C(-0.0794) H18A(0.2074) H18B(0.2143) H18C(0.214) H22(0.2103) H23(0.2844)
 H25(0.2853) H26(0.2111) H31(0.2065) H32(0.2776) H34(0.2592) H35(0.1869)
 H39(0.1746) H40(0.1002) H42(0.2165) H43(0.2917) H52A(0.1696) H52B(0.1763)
 H52C(0.1758) H53A(-0.0665) H53B(-0.0707) H53C(-0.1306) H55A(-0.0362) H55B(-
 0.0922) H55C(-0.107) H59(-0.2986) H60(-0.421) H62(-0.4318) H63(-0.3074)
 H67(0.2275) H68(0.2982) H70(0.1782) H71(0.1062) H73A(0.6209) H73B(0.5945)
 H73C(0.634) H74A(0.4647) H74B(0.5441) H74C(0.5125) H75(0.4474) H76A(0.7013)
 H76B(0.6635) H76C(0.654) H77A(0.5853) H77B(0.6528) H77C(0.5762) H78(0.5012)
 H81A(0.5501) H81B(0.5462) H81C(0.6205) H82A(0.6113) H82B(0.6173) H82C(0.6605)
 H83(0.4636) H84A(0.6691) H84B(0.6463) H84C(0.5915) H85A(0.6392) H85B(0.6922)
 H85C(0.6578) H86(0.513)
;
_olex2_submission_special_instructions 'No special instructions were received'