Interactions between 2,4-bis-pteridine-1,5-benzodiazepine and group 12 dihalides: synthesis, spectral and XRD structural studies and theoretical calculations.
Illán-Cabeza, Nuria A; Jiménez-Pulido, Sonia B; Hueso-Ureña, Francisco; Peña-Ruiz, Tomás; Quirós-Olozábal, Miguel; Moreno-Carretero, Miguel N; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17896–17909; doi:10.1039/c6dt03583c

data_7040864
_publ_section_title
;
 Interactions between 2,4-bis-pteridine-1,5-benzodiazepine and group 12
 dihalides: synthesis, spectral and XRD structural studies and theoretical
 calculations.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17896
_journal_page_last               17909
_journal_paper_doi               10.1039/c6dt03583c
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H28 Hg I2 N10 O4'
_chemical_formula_sum            'C28 H28 Hg I2 N10 O4'
_chemical_formula_weight         1022.99
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-24 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.031(5)
_cell_length_b                   15.388(5)
_cell_length_c                   14.032(5)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3.5
_cell_volume                     3245.6(19)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23670
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         3.931
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    6.695
_exptl_absorpt_correction_T_max  0.6164
_exptl_absorpt_correction_T_min  0.1255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2.10, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details
; 
 Flack x determined using 2447 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.073(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                6089
_reflns_number_total             7257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03583c2.cif
_cod_data_source_block           hgdlmbzd
_cod_depositor_comments
'Adding full bibliography for 7040859--7040866.cif.'
_cod_database_code               7040864
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.125
_shelx_estimated_absorpt_t_max   0.616
_shelx_res_checksum              45975