Conformational analysis and synthetic approaches to polydentate perhydro-diazepine ligands for the complexation of gallium(iii).
Parker, David; Waldron, Bradley P.; Organic & biomolecular chemistry 11 (2013) 2827–2838; doi:10.1039/c3ob40287h

data_7152907
_publ_section_title
;
 Conformational analysis and synthetic approaches to polydentate
 perhydro-diazepine ligands for the complexation of gallium(iii).
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2827
_journal_page_last               2838
_journal_paper_doi               10.1039/c3ob40287h
_journal_volume                  11
_journal_year                    2013
_chemical_formula_moiety         'C23 H35 N3 O6'
_chemical_formula_sum            'C23 H35 N3 O6'
_chemical_formula_weight         449.54
_chemical_melting_point          357(6)
_chemical_name_systematic
;
tert-Butyl 2,2'-(6-nitro-6-phenyl-1,4-diazepane-1,4-diyl)diacetate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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Olex2 1.1-beta
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.329(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3378(19)
_cell_length_b                   11.5579(10)
_cell_length_c                   10.3203(9)
_cell_measurement_reflns_used    790
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.4600
_cell_measurement_theta_min      2.6160
_cell_volume                     2503.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
1 omega -103.00 -74.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- -26.1867 165.0000 147.0000 29
2 omega -88.00 47.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- -26.1867 0.0000 90.0000 135
3 omega 57.00 89.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 179.0000 30.0000 32
4 omega 61.00 103.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 179.0000 -90.0000 42
5 omega 50.00 103.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 26.9679 -165.0000 -55.0000 53
6 omega -96.00 -37.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- -26.1867 -77.0000 30.0000 59
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.0231851000
_diffrn_orient_matrix_UB_12      -0.0440000000
_diffrn_orient_matrix_UB_13      0.0173170000
_diffrn_orient_matrix_UB_21      -0.0245687000
_diffrn_orient_matrix_UB_22      -0.0418002000
_diffrn_orient_matrix_UB_23      -0.0037504000
_diffrn_orient_matrix_UB_31      0.0010320000
_diffrn_orient_matrix_UB_32      -0.0088930000
_diffrn_orient_matrix_UB_33      -0.0675991000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.1564
_diffrn_reflns_av_unetI/netI     0.2183
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15496
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         0.9042
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_type              'sealed tube'
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.338
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.2327
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.2425
_reflns_number_gt                1948
_reflns_number_total             5463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ob40287h.txt
_cod_data_source_block           10_12srv031
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '78-90 C' was changed to '357(6)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7152907
_chemical_oxdiff_formula         'C23 H35 N3 O6'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44