Fine-tuning polyoxometalate non-linear optical chromophores: a molecular electronic "Goldilocks" effect.
Al-Yasari, Ahmed; Spence, Philip; El Moll, Hani; Van Steerteghem, Nick; Horton, Peter N.; Brunschwig, Bruce S.; Clays, Koen; Fielden, John; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10415–10419; doi:10.1039/c8dt01491d

data_7046865
_publ_section_title
;
 Fine-tuning polyoxometalate non-linear optical chromophores: a molecular
 electronic &quot;Goldilocks&quot; effect.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10415
_journal_page_last               10419
_journal_paper_doi               10.1039/c8dt01491d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C26 H18 Mo6 N2 O18, 2 (C16 H36 N), 0.25 (C2 H3 N)'
_chemical_formula_sum            'C58.5 H90.75 Mo6 N4.25 O18'
_chemical_formula_weight         1717.24
_chemical_properties_physical    Moisture-sensitive
_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
;
2018-04-16 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7634(2)
_cell_length_b                   32.5035(4)
_cell_length_c                   30.9114(6)
_cell_measurement_reflns_used    57564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6480
_cell_measurement_theta_min      2.3070
_cell_volume                     16842.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            165986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.992
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72368
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       Block
_exptl_crystal_F_000             6940
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 13251 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1802
_refine_ls_number_reflns         38580
_refine_ls_number_restraints     1386
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1167P)^2^+36.4219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2178
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                32626
_reflns_number_total             38580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01491d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7046864--7046865.cif.'
_cod_original_formula_sum        'C58.50 H90.75 Mo6 N4.25 O18'
_cod_database_code               7046865
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_res_checksum              59865