Unusual Intramolecular CH...O Hydrogen Bonding Interaction between Sterically Bulky Amide and Uranyl oxygen
Kannan, Shanmugaperumal; Kumar, Mukesh; Sadhu, Biswajit; Madhavan, Jaccob; Sundararajan, Mahesh; Dalton Transactions  (2017) –; doi:10.1039/C7DT02760E

data_7044720
_publ_section_title
;
 Unusual Intramolecular CH...O Hydrogen Bonding Interaction between
 Sterically Bulky Amide and Uranyl oxygen
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT02760E
_journal_year                    2017
_chemical_formula_sum            'C43 H48 N3 Ni O'
_chemical_formula_weight         681.55
_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_method           SHELXL-2014/7
_audit_update_record
;
2016-08-08 deposited with the CCDC.
2017-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.532(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4481(17)
_cell_length_b                   9.4949(9)
_cell_length_c                   27.331(4)
_cell_measurement_reflns_used    25337
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.123
_cell_measurement_theta_min      1.533
_cell_volume                     3645.3(8)
_computing_cell_refinement
;      
'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
;
_computing_data_collection
;      
'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
;
_computing_data_reduction
;      
'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1314
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.589
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       Block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0004(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+5.4758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2367
_reflns_number_total             3213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02760e1.cif
_cod_data_source_block           Ni_NNN_OH
_cod_original_cell_volume        3645.2(8)
_cod_database_code               7044720
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              45456