Synthesis and characterization of inorganic-organic hybrid gallium selenides.
Ewing, Sarah J.; Vaqueiro, Paz; Inorganic chemistry 53 (2014) 8845–8847; doi:10.1021/ic5011314

data_4340690
_publ_section_title
;
 Synthesis and characterization of inorganic-organic hybrid gallium
 selenides.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8845
_journal_page_last               8847
_journal_paper_doi               10.1021/ic5011314
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C24.00 H52.00 Ga6 N8 O1 Se9'
_chemical_formula_sum            'C24 H52 Ga6 N8 O Se9'
_chemical_formula_weight         1597.70
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1919(7)
_cell_length_b                   19.6774(12)
_cell_length_c                   20.8361(13)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4588.7(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63184
_diffrn_reflns_theta_full        26.390
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         1.423
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.643
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008.017
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.0007543
_refine_ls_shift/su_mean         0.0000344
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.227 0.164 0.101 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0861
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0385
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2980
_reflns_number_total             4700
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.15
_oxford_diffrn_Wilson_scale      1687.92
_oxford_refine_ls_r_factor_ref   0.0369
_oxford_refine_ls_scale          0.03127(5)
_oxford_reflns_number_all        4682
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic5011314_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340690--4340691.cif.
;
_cod_original_sg_symbol_H-M      'P n n a '
_cod_original_formula_sum        'C24.00 H52.00 Ga6 N8 O1 Se9'
_cod_database_code               4340690
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT GA(1, U'S) UNTIL SE (9) 
EQUIV PART(1001, U[ISO]) PART(1002, U[ISO]) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
CONT N(24, U'S) UNTIL O(32) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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SAME C(20) C(18) C(19) C(12) N(13) AND 
CONT C(21) C(22) C(17) C(16) C(14) N(15) 
DIST 1.47, 0.01 = N(24) TO C(25), N(30) TO C(31) 
DIST 1.54, 0.01 = C(25) TO C(26), C(27) TO C(26) 
DIST 1.54, 0.01 = C(28) TO C(27), C(29) TO C(28) 
DIST 1.54, 0.01 = C(30) TO C(29), C(30) TO C(25) 
DIST 1.47, 0.01 = C(12) TO N(13), C(11) TO N(10) 
DIST 1.54, 0.01 = C(12) TO C(11), C(20) TO C(11) 
DIST 1.54, 0.01 = C(23) TO C(20), C(23) TO C(18) 
DIST 1.54, 0.01 = C(19) TO C(18), C(19) TO C(12) 
DIST 1.47, 0.01 = C(14) TO C(15) 
DIST 1.54, 0.01 = C(11) TO C(21), C(22) TO C(21) 
DIST 1.54, 0.01 = C(22) TO C(21), C(22) TO C(17) 
DIST 1.54, 0.01 = C(17) TO C(16), C(16) TO C(14) 
DIST 1.54, 0.01 = C(11) TO C(14) 
END                                                                             
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