Dipicolinate Complexes of Gallium(III) and Lanthanum(III).
Weekes, David M.; Ramogida, Caterina F.; Jaraquemada-Peláez, Maria de Guadalupe; Patrick, Brian O.; Apte, Chirag; Kostelnik, Thomas I.; Cawthray, Jacqueline F.; Murphy, Lisa; Orvig, Chris; Inorganic chemistry 55 (2016) 12544–12558; doi:10.1021/acs.inorgchem.6b02357

data_4349308
_publ_section_title
;
 Dipicolinate Complexes of Gallium(III) and Lanthanum(III).
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12544
_journal_page_last               12558
_journal_paper_doi               10.1021/acs.inorgchem.6b02357
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C16 H14 Ga N3 O7, 2(H2 O)'
_chemical_formula_sum            'C16 H18 Ga N3 O9'
_chemical_formula_weight         466.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2013-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.9305(18)
_cell_length_b                   35.941(2)
_cell_length_c                   7.0749(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.61
_cell_volume                     7865.0(8)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12536
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         1.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0617 before and 0.0504 after correction.
 The Ratio of minimum to maximum transmission is 0.86.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0663 before and 0.0553 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 108254 reflections, Rint = 0.0824
 (38300 with I > 3sig(I), Rint = 0.0518)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       prism
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         11334
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+80.0424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8137
_reflns_number_total             11334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02357_si_004.cif
_cod_data_source_block           co453
_cod_original_cell_volume        7865.1(8)
_cod_database_code               4349308
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
3.a Free rotating group:
 O15(H15A,H15B,O18,H18A,H18B), O16(H16C,H16D,O17,H17A,H17B)
3.b Rotating group:
 O7(H7C,H7D), O14(H14A,H14B)
3.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B),
 C32(H32A,H32B)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C19(H19), C20(H20),
 C21(H21), C26(H26), C27(H27), C28(H28)
;
_shelx_res_checksum              83551
_shelx_hkl_checksum              70774