Dicyanoaurate-based heterobimetallic uranyl coordination polymers.
Brown, Matthew L.; Ovens, Jeffrey S.; Leznoff, Daniel B.; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00942a

data_7042989
_publ_section_title
;
 Dicyanoaurate-based heterobimetallic uranyl coordination polymers.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00942a
_journal_year                    2017
_chemical_formula_moiety
'C30 H22 N7 O8 U2, 2(C2 H3 N), Au C2 N2'
_chemical_formula_sum            'C36 H28 Au N11 O8 U2'
_chemical_formula_weight         1415.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.146(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2358(7)
_cell_length_b                   24.0833(18)
_cell_length_c                   14.6019(9)
_cell_measurement_reflns_used    2309
_cell_measurement_temperature    149.97
_cell_measurement_theta_max      69.39
_cell_measurement_theta_min      3.67
_cell_volume                     3985.4(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
'Olex2 (Dolomanov et al., 2009), ShelXle (H\"ubschle et al., 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'XT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.97
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12620
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         3.671
_diffrn_source
'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    29.958
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.1092 before and 0.0674 after correction. 
The Ratio of minimum to maximum transmission is 0.6709. 
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_preparation       'Solvothermal from MeCN'
_exptl_crystal_recrystallization_method
'Solvothermal from MeCN. Note: Crystal size is approximate:crystal was hard to see on camera due to colour.''
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.867
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2951
_reflns_number_total             3627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_depositor_comments
;

2018-07-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H56 Au2 N22 O16 U4'
_cod_original_formula_weight         2831.44
_cod_original_formula_moiety
'2(C30 H22 N7 O8 U2), 4(C2 H3 N), 2(Au C2 N2)'
_cod_original_formula_units_Z            2
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           terpy
_cod_database_code               7042989
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C8(H8), C13(H13), C10(H10), C14(H14),
 C15(H15), C16(H16), C5(H5)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              89637
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2015-01-07
_olex2_date_sample_data_collection 2015-01-06
_olex2_date_sample_submission    2015-01-06
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMount using parabar oil'
_olex2_submission_original_sample_id MLB3_38