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_4340691
_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         'C18 H38.00 Ga4 N6 Se6'
_chemical_formula_sum            'C18 H38 Ga4 N6 Se6'
_chemical_formula_weight         1091.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 105.253(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2095(8)
_cell_length_b                   11.0633(6)
_cell_length_c                   21.2998(11)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3230.5(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.986
_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  0.054
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6539
_diffrn_reflns_theta_full        25.613
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         1.554
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.080
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064.001
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0507
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.0080988
_refine_ls_shift/su_mean         0.0005599
_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: 
 0.462 0.185 0.250 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0663
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0530
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5198
_reflns_number_total             6539
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.73
_oxford_diffrn_Wilson_scale      462.12
_oxford_refine_ls_r_factor_ref   0.0550
_oxford_refine_ls_scale          0.05411(9)
_oxford_reflns_number_all        6514
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic5011314_si_001.cif
_cod_data_source_block           2
_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 21/n '
_cod_original_formula_sum        'C18 H38.00 Ga4 N6 Se6'
_cod_database_code               4340691
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONTINUE GA(1, U'S) UNTIL SE(10) 
CONTINUE N(11, U[ISO]) UNTIL C(35) 
EQUIV PART(1001, U[ISO]) PART(1002, U[ISO]) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(1003, U[ISO]) PART(1004, U[ISO]) 
EQUIV PART(1003,OCC) PART(1004,OCC) 
WEIGHT -1 PART(1003,OCC) 
EQUIV PART(1005, U[ISO]) PART(1006, U[ISO]) 
EQUIV PART(1005,OCC) PART(1006,OCC) 
WEIGHT -1 PART(1005,OCC) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME N(39) C(37) C(35) C(32) C(31) C(9) AND 
CONT N(38) C(36) C(34) C(33) C(30) C(28) 
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) 
SAME C(18) C(2) AND C(1) C(13) 
SAME C(8) AND C(16) 
SAME C(11) AND C(17) 
DIST 1.47, 0.01 = C(28) TO N(27), N(38) TO C(36) 
DIST 1.47, 0.01 = C(37) TO N(39) 
DIST 1.54, 0.01 = C(37) TO C(28), C(29) TO C(28) 
DIST 1.54, 0.01 = C(36) TO C(28), C(30) TO C(29) 
DIST 1.54, 0.01 = C(33) TO C(30), C(33) TO C(34) 
DIST 1.54, 0.01 = C(34) TO C(36), C(29) TO C(31) 
DIST 1.47, 0.01 = C(26) TO N(19), N(21) TO C(20) 
DIST 1.54, 0.01 = C(26) TO C(21), C(26) TO C(25) 
DIST 1.54, 0.01 = C(25) TO C(24), C(24) TO C(23) 
DIST 1.54, 0.01 = C(23) TO C(22), C(22) TO C(21) 
DIST 1.47, 0.01 = C(18) TO N(11), N(13) TO C(12) 
DIST 1.54, 0.01 = C(18) TO C(13), C(18) TO C(17) 
DIST 1.54, 0.01 = C(17) TO C(16), C(16) TO C(15) 
DIST 1.54, 0.01 = C(15) TO C(14), C(14) TO C(13) 
DIST 1.54, 0.01 = C(35) TO C(32), C(32) TO C(31) 
DIST 1.47, 0.01 = C(13) TO N(12), C(18) TO N(11) 
DIST 1.54, 0.01 = C(18) TO C(17), C(1) TO C(17) 
DIST 1.54, 0.01 = C(14) TO C(13), C(1) TO C(17) 
DIST 1.47, 0.01 = C(9) TO N(27), N(38) TO C(36) 
DIST 1.54, 0.01 = C(8) TO C(17), C(8) TO C(15) 
DIST 1.54, 0.01 = C(35) TO C(37), C(33) TO C(34) 
DIST 1.54, 0.01 = C(34) TO C(36), C(16) TO C(11) 
DIST 1.54, 0.01 = C(18) TO C(11) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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