Donor-acceptor organo-imido polyoxometalates: high transparency, high activity redox-active NLO chromophores.
Al-Yasari, Ahmed; Van Steerteghem, Nick; El Moll, Hani; Clays, Koen; Fielden, John; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2818–2822; doi:10.1039/c6dt00115g

data_7038046
_publ_section_title
;
 Donor-acceptor organo-imido polyoxometalates: high transparency, high
 activity redox-active NLO chromophores.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2818
_journal_page_last               2822
_journal_paper_doi               10.1039/c6dt00115g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C18 H12 Mo6 N2 O18, 2(C16 H36 N)'
_chemical_formula_sum            'C50 H84 Mo6 N4 O18'
_chemical_formula_weight         1604.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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
;
2015-09-29 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5590(11)
_cell_length_b                   17.7832(13)
_cell_length_c                   19.6079(14)
_cell_measurement_reflns_used    30611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     6122.7(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42376
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.576
_diffrn_reflns_theta_min         2.320
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.8635
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 1823 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         14052
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.826
_reflns_friedel_fraction_full    0.996
_reflns_friedel_fraction_max     0.987
_reflns_number_gt                5819
_reflns_number_total             14052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00115g2.cif
_cod_data_source_block           NBu4-2
_cod_depositor_comments
'Adding full bibliography for 7038045--7038047.cif.'
_cod_database_code               7038046
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              26184