Phospha Derivatives of Tris(2-aminoethyl)amine (tren) and Tris(3-aminopropyl)amine (trpn): Synthesis and Complexation Studies with Group 4 Metals
Sietzen, Malte; Batke, Sonja; Merz, Lukas; Wadepohl, Hubert; Ballmann, Joachim; Organometallics 34 (2015) 1118–; doi:10.1021/acs.organomet.5b00065

data_1518841
_publ_section_title
;
 Phospha Derivatives of Tris(2-aminoethyl)amine (tren) and
 Tris(3-aminopropyl)amine (trpn): Synthesis and Complexation Studies with
 Group 4 Metals
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1118
_journal_paper_doi               10.1021/acs.organomet.5b00065
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H33 F3 N3 O3 P S Zr'
_chemical_formula_sum            'C28 H33 F3 N3 O3 P S Zr'
_chemical_formula_weight         670.82
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_jb13
_audit_creation_date
;
'Tue May 27 15:24:51 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record             '20.01.2015 14:58:46 CET UTC+01:00  encif 1.29'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.62850(16)
_cell_length_b                   10.81736(10)
_cell_length_c                   30.9896(3)
_cell_measurement_reflns_used    101155
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.5370
_cell_measurement_theta_min      3.7630
_cell_volume                     5909.53(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -26.00   -1.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        6.0000   80.0000  119.5849 50

  2 omega  -45.00    1.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000 -143.2484 92

  3 omega   56.00   83.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   19.0000 -150.0000 54

  4 omega   24.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  112.4010 52

  5 omega   48.00   75.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -120.0000 54

  6 omega    6.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  120.0000 162

  7 omega    2.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000    0.0000 94

  8 omega   -2.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -150.0000 178

  9 omega  -52.00  -23.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 58

 10 omega    9.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 80

 11 omega   24.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   30.0000 50

 12 omega    0.00   33.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   30.0000 66

 13 omega   45.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   30.0000 78

 14 omega  -38.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -30.0000 174

 15 omega   24.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000 -143.2484 52

 16 omega   42.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   30.0000 90

 17 omega  -12.00   79.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  -60.0000 182

 18 omega  -51.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   90.0000 200

 19 omega   24.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 50

 20 omega  -46.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  -86.4153 192

 21 omega  -50.00   40.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000  -90.0000 180

 22 omega  -50.00   40.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000   90.0000 180

 23 omega   -7.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000 -120.0000 196

 24 omega   -3.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   60.0000 180

 25 omega  -50.00   40.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000    0.0000 180

 26 omega  -50.00   40.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000  150.0000 180

 27 omega   -3.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -180.0000 180

 28 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 202

 29 omega   -3.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -30.0000 180

 30 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   60.0000 202

 31 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -60.0000 202

 32 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 202

 33 omega  -47.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  -86.4153 194

 34 omega   -3.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   90.0000 180

 35 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -30.0000 202

 36 omega  -12.00   89.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  -90.0000 202

 37 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   90.0000 202

 38 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 202

 39 omega  -54.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380    0.0000    0.0000 290

 40 omega  -54.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380    0.0000  120.0000 290

 41 omega  -54.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380    0.0000  240.0000 290

 42 phi      0.00  120.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.5380    0.0000     -     240

 43 phi      0.00  119.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
  18.5380   18.5380  -20.0000     -     238

 44 omega  -52.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000    0.0000 202

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0040946000
_diffrn_orient_matrix_UB_12      0.0372461000
_diffrn_orient_matrix_UB_13      -0.0186964000
_diffrn_orient_matrix_UB_21      -0.0069887000
_diffrn_orient_matrix_UB_22      -0.0536601000
_diffrn_orient_matrix_UB_23      -0.0125441000
_diffrn_orient_matrix_UB_31      -0.0394090000
_diffrn_orient_matrix_UB_32      0.0056706000
_diffrn_orient_matrix_UB_33      0.0041398000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            401672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.911
_diffrn_reflns_theta_min         3.234
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.571
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 6367 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         15293
_refine_ls_number_restraints     416
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+11.0893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                14782
_reflns_number_total             15293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00065_si_002.cif
_cod_data_source_block           ba_jb13
_cod_depositor_comments
'Adding full bibliography for 1518840--1518841.cif.'
_cod_original_cell_volume        5909.52(10)
_cod_database_code               1518841
_audit_block_refno               2054
_audit_block_usercomment         'jb113, irregular, yellow'
_chemical_oxdiff_formula         'C28 H33 N3 F3 O3 S P Zr'
_chemical_oxdiff_usercomment     'jb113, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.947
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N51A-C60A \\sim N51B-C60B
 with sigma of 0.02
 N52A-C66A \\sim N52B-C66B
 with sigma of 0.02
 Zr51-N51A \\sim Zr51-N51B
 with sigma of 0.02
 Zr51-N52A \\sim Zr51-N52B
 with sigma of 0.02
 P51-C51A \\sim P51-C51B \\sim P51-C54A \\sim P51-C54B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1A \\sim O2A \\sim O3A \\sim C28A \\sim F1A \\sim F2A \\sim F3A \\sim S1B
\\sim O2B \\sim O3B \\sim C28B \\sim F1B \\sim F2B \\sim F3B: within 0.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C57 \\sim C58 \\sim C59 \\sim C51A \\sim C52A \\sim C53A \\sim C60A \\sim C61A
\\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim C51B \\sim C52B \\sim C53B
\\sim C60B \\sim C61B \\sim C62B \\sim C63B \\sim C64B \\sim C65B \\sim C54A
\\sim C55A \\sim C56A \\sim C66A \\sim C67A \\sim C68A \\sim C69A \\sim C70A
\\sim C71A \\sim C54B \\sim C55B \\sim C56B \\sim C66B \\sim C67B \\sim C68B
\\sim C69B \\sim C70B \\sim C71B \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim
C76 \\sim C77 \\sim C78 \\sim C18 \\sim C22 \\sim C26 \\sim C16 \\sim C20 \\sim
C24 \\sim C1 \\sim C2 \\sim C3 \\sim C15 \\sim C4 \\sim C17 \\sim C5 \\sim C19
\\sim C6 \\sim C21 \\sim C7 \\sim C23 \\sim C8 \\sim C25 \\sim C9 \\sim C27
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C28A \\sim C28B: within
0.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N53 \\sim N51A \\sim N51B \\sim N52A \\sim N52B \\sim N2 \\sim N3 \\sim N1:
within 0.7A with sigma of 0.01 and sigma for terminal atoms of 0.04
Uanis(S1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq,
Uanis(S1B) \\sim Ueq, Uanis(O2B) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(C28B)
\\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F3B) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.05
4. Rigid body (RIGU) restrains
 N51A, C60A, C61A, C62A, C63A, C64A, C65A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N51B, C60B, C61B, C62B, C63B, C64B, C65B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N52A, C66A, C67A, C68A, C69A, C70A, C71A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N52B, C66B, C67B, C68B, C69B, C70B, C71B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N51A, C51A, C52A, C53A, C60A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N51B, C51B, C52B, C53B, C60B}
{N52A, C54A, C55A, C56A, C66A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N52B, C54B, C55B, C56B, C66B}
{S1A, O2A, O3A, C28A, F1A, F2A, F3A} sigma for 1-2: 0.01, 1-3: 0.01
as
{S1B, O2B, O3B, C28B, F1B, F2B, F3B}
6. Others
 Sof(N51B)=Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=
 Sof(C53B)=Sof(H53C)=Sof(H53D)=Sof(C60B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=
 Sof(H62B)=Sof(C63B)=Sof(H63B)=Sof(C64B)=Sof(H64B)=Sof(C65B)=Sof(H65B)=Sof(S1B)=
 Sof(O2B)=Sof(O3B)=Sof(C28B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(N51A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=
 Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(C60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=
 Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(S1A)=
 Sof(O2A)=Sof(O3A)=Sof(C28A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(N52B)=Sof(C54B)=Sof(H54C)=Sof(H54D)=Sof(C55B)=Sof(H55C)=Sof(H55D)=
 Sof(C56B)=Sof(H56C)=Sof(H56D)=Sof(C66B)=Sof(C67B)=Sof(H67B)=Sof(C68B)=
 Sof(H68B)=Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(H70B)=Sof(C71B)=Sof(H71B)=1-FVAR(2)
 Sof(N52A)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(C55A)=Sof(H55A)=Sof(H55B)=
 Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(C66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=
 Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70A)=Sof(C71A)=Sof(H71A)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C51A(H51A,H51B), C52A(H52A,
 H52B), C53A(H53A,H53B), C51B(H51C,H51D), C52B(H52C,H52D), C53B(H53C,H53D),
 C54A(H54A,H54B), C55A(H55A,H55B), C56A(H56A,H56B), C54B(H54C,H54D), C55B(H55C,
 H55D), C56B(H56C,H56D), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
7.b Aromatic/amide H refined with riding coordinates:
 C61A(H61A), C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C61B(H61B),
 C62B(H62B), C63B(H63B), C64B(H64B), C65B(H65B), C67A(H67A), C68A(H68A),
 C69A(H69A), C70A(H70A), C71A(H71A), C67B(H67B), C68B(H68B), C69B(H69B),
 C70B(H70B), C71B(H71B), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C18(H18), C26(H26), C20(H20), C24(H24), C15(H15), C17(H17), C19(H19), C21(H21),
  C23(H23), C25(H25), C27(H27), C11(H11), C12(H12), C13(H13), C14(H14)
7.c Fitted hexagon refined as free rotating group:
 C60A(C61A,C62A,C63A,C64A,C65A), C60B(C61B,C62B,C63B,C64B,C65B), C66A(C67A,
 C68A,C69A,C70A,C71A), C66B(C67B,C68B,C69B,C70B,C71B)
;
_shelx_res_checksum              89406
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            17.62992(13)
_cell_oxdiff_length_b            10.81819(9)
_cell_oxdiff_length_c            30.9847(3)
_cell_oxdiff_angle_alpha         90.0085(7)
_cell_oxdiff_angle_beta          90.0670(6)
_cell_oxdiff_angle_gamma         89.9791(6)
_cell_oxdiff_volume              5909.53(8)
_cell_oxdiff_measurement_reflns_used 101155