Crystallographic and solution NMR structural analyses of four hexacoordinated gallium(iii) complexes based on ligands derived from 6-amino-perhydro-1,4-diazepine.
Parker, David; Waldron, Bradley P.; Yufit, Dmitry S.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8001–8008; doi:10.1039/c3dt50287b

data_7021422
_publ_section_title
;
 Crystallographic and solution NMR structural analyses of four
 hexacoordinated gallium(iii) complexes based on ligands derived from
 6-amino-perhydro-1,4-diazepine.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8001
_journal_page_last               8008
_journal_paper_doi               10.1039/c3dt50287b
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H26 Ga N3 O6'
_chemical_formula_sum            'C20 H26 Ga N3 O6'
_chemical_formula_weight         474.16
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled Nov 5 2012 18:22:26, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3312(7)
_cell_length_b                   13.9288(12)
_cell_length_c                   19.6479(19)
_cell_measurement_reflns_used    4522
_cell_measurement_temperature    100
_cell_measurement_theta_max      57.74
_cell_measurement_theta_min      3.89
_cell_volume                     2006.3(3)
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Pt-135'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'Bruker Proteum'
_diffrn_measurement_device_type  'Bruker Proteum CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54188
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8432
_diffrn_reflns_theta_full        57.47
_diffrn_reflns_theta_max         57.47
_diffrn_reflns_theta_min         4.50
_diffrn_source                   'Microstar rotating anode'
_diffrn_source_target            Cu
_diffrn_source_type              'rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.262
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.5136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0896 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.6835.
The \l/2 correction factor is 0.0015.
;
_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    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                2304
_reflns_number_total             2584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50287b.txt
_cod_data_source_block           GaL4
_cod_database_code               7021422
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
{H1a,H1b} of C1, {H2a,H2b} of C2, H20 of C20, H3 of N3, H6 of C6, H8 of C8,
H10 of C10, H16 of C16, H17 of C17, H18 of C18, H19 of C19, {H3a,H3b} of C3,
{H5a,H5b} of C5
At 1.5 times of:
{H12a,H12b,H12c} of C12, {H13a,H13b,H13c} of C13, {H14a,H14b,H14c} of C14
2.a Ternary CH refined with riding coordinates:
N3(H3), C6(H6), C8(H8), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C5(H5a,H5b)
2.c Aromatic/amide H refined with riding coordinates:
C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c)
;