A versatile hard-soft N/S-ligand for metal coordination and cluster formation.
Benson, Callum G. M.; Plajer, Alex J.; García-Rodríguez, Raúl; Bond, Andrew D.; Singh, Sanjay; Gade, Lutz H.; Wright, Dominic S.; Chemical communications (Cambridge, England) 52 (2016) 9683–9686; doi:10.1039/c6cc04805f

data_7124812
_publ_section_title
;
 A versatile hard-soft N/S-ligand for metal coordination and cluster
 formation.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9683
_journal_page_last               9686
_journal_paper_doi               10.1039/c6cc04805f
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C96 H209 N16 Na17 O8 P16 S17'
_chemical_formula_sum            'C96 H209 N16 Na17 O8 P16 S17'
_chemical_formula_weight         3147.15
_space_group_crystal_system      tetragonal
_space_group_IT_number           103
_space_group_name_Hall           'P 4 -2c'
_space_group_name_H-M_alt        'P 4 c c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-19 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7918(2)
_cell_length_b                   23.7918(2)
_cell_length_c                   37.5449(6)
_cell_measurement_reflns_used    102364
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.00
_cell_volume                     21252.3(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            39076
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        22.481
_diffrn_reflns_theta_max         22.481
_diffrn_reflns_theta_min         3.531
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       block
_exptl_crystal_F_000             6640
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;
TITL dw_k3_0045 in P4cc
CELL   23.7918   23.7918   37.5449     90.00     90.00     90.00
SPGR P4cc
C101 0.986 0.201 0.086 !       2.68 eA-3
C102 0.655 0.051 0.672 !       2.67 eA-3
C103 0.321 0.662 0.400 !       2.67 eA-3
C104 0.012 0.853 0.093 !       2.65 eA-3
C105 0.648 0.285 0.885 !       2.59 eA-3
C106 0.015 0.540 0.283 !       2.59 eA-3
C107 0.398 0.367 0.373 !       2.50 eA-3
C108 0.912 0.596 0.618 !       2.50 eA-3
C109 0.642 0.062 0.647 !       2.48 eA-3
C110 0.259 0.379 0.881 !       2.46 eA-3
C111 0.813 0.012 0.101 !       2.46 eA-3
C112 0.634 0.249 0.891 !       2.40 eA-3
C113 0.383 0.622 0.382 !       2.37 eA-3
C114 0.054 0.811 0.625 !       2.34 eA-3
C115 0.047 0.502 0.463 !       2.34 eA-3
C116 0.032 0.514 0.992 !       2.33 eA-3
C117 0.986 0.476 0.251 !       2.31 eA-3
C118 0.444 0.036 0.271 !       2.31 eA-3
C119 0.414 0.315 0.376 !       2.30 eA-3
C120 0.063 0.549 0.093 !       2.24 eA-3
C121 0.069 0.643 0.115 !       2.24 eA-3
C122 0.984 0.532 0.125 !       2.23 eA-3
C123 0.697 0.441 0.357 !       2.20 eA-3
C124 0.347 0.639 0.881 !       2.20 eA-3
C125 0.937 0.856 0.132 !       2.19 eA-3
C126 0.500 0.996 0.235 !       2.16 eA-3
C127 0.039 0.272 0.093 !       2.13 eA-3
C128 0.462 0.984 0.805 !       2.10 eA-3
C129 0.046 0.604 0.141 !       2.10 eA-3
C130 1.001 0.475 0.829 !       2.09 eA-3
C131 0.616 0.694 0.368 !       2.07 eA-3
C132 0.345 0.945 0.625 !       2.07 eA-3
C133 0.963 0.690 0.080 !       2.07 eA-3
C134 0.500 0.504 0.398 !       2.01 eA-3
C135 0.497 0.981 0.946 !       2.00 eA-3
C136 0.522 0.032 0.835 !       2.00 eA-3
C137 0.773 0.391 0.399 !       1.96 eA-3
C138 0.958 0.144 0.618 !       1.95 eA-3
C139 0.227 0.037 0.601 !       1.94 eA-3
C140 0.766 0.587 0.885 !       1.94 eA-3
C141 0.986 0.763 0.079 !       1.93 eA-3
C142 0.115 0.970 0.125 !       1.92 eA-3
C143 0.092 0.195 0.133 !       1.92 eA-3
C144 0.430 0.015 0.820 !       1.92 eA-3
C145 0.021 0.425 0.822 !       1.91 eA-3
C146 0.469 0.029 0.496 !       1.91 eA-3
C147 0.347 0.447 0.857 !       1.91 eA-3
C148 0.031 0.440 0.749 !       1.89 eA-3
C149 0.500 0.500 0.773 !       1.88 eA-3
C150 1.000 0.502 0.492 !       1.88 eA-3
C151 0.039 0.375 0.625 !       1.88 eA-3
C152 0.500 0.498 0.844 !       1.87 eA-3
C153 0.044 0.375 0.571 !       1.86 eA-3
C154 0.548 0.053 0.812 !       1.85 eA-3
C155 0.736 0.561 0.843 !       1.85 eA-3
C156 0.492 0.999 0.139 !       1.85 eA-3
C157 0.429 0.260 0.374 !       1.83 eA-3
C158 0.750 0.008 0.593 !       1.83 eA-3
C159 1.000 0.496 0.116 !       1.82 eA-3
C160 0.212 0.359 0.923 !       1.81 eA-3
C161 0.429 0.885 0.437 !       1.81 eA-3
C162 0.032 0.340 0.609 !       1.81 eA-3
C163 0.992 0.430 0.648 !       1.80 eA-3
Q164 0.030 0.702 0.540 !       1.79 eA-3
C165 0.369 0.689 0.398 !       1.78 eA-3
C166 0.422 0.252 0.290 !       1.77 eA-3
C167 0.650 0.006 0.562 !       1.75 eA-3
C168 0.428 0.367 0.398 !       1.75 eA-3
C169 0.438 0.617 0.382 !       1.73 eA-3
C170 0.686 0.988 0.125 !       1.72 eA-3
C171 0.500 0.495 0.930 !       1.72 eA-3
C172 0.008 0.883 0.609 !       1.71 eA-3
C173 0.664 0.355 0.351 !       1.70 eA-3
C174 0.056 0.441 0.623 !       1.70 eA-3
C175 0.708 1.001 0.578 !       1.70 eA-3
C176 0.224 0.545 0.361 !       1.70 eA-3
C177 0.087 0.604 0.068 !       1.68 eA-3
Q178 0.891 0.420 0.049 !       1.68 eA-3
C179 0.556 0.713 0.290 !       1.67 eA-3
C180 0.446 0.932 0.821 !       1.67 eA-3
C181 0.648 0.671 0.921 !       1.67 eA-3
C182 0.053 0.490 0.642 !       1.63 eA-3
C183 0.499 0.996 0.968 !       1.62 eA-3
C184 0.915 0.834 0.116 !       1.62 eA-3
C185 0.500 0.505 0.453 !       1.62 eA-3
C186 0.025 0.673 0.133 !       1.61 eA-3
C187 0.078 0.779 0.617 !       1.61 eA-3
C188 0.318 1.004 0.060 !       1.60 eA-3
C189 0.663 0.715 0.890 !       1.59 eA-3
C190 0.422 0.973 0.843 !       1.58 eA-3
C191 0.999 0.904 0.616 !       1.58 eA-3
C192 0.704 0.024 0.534 !       1.58 eA-3
C193 0.367 0.977 0.616 !       1.57 eA-3
C194 0.687 0.101 0.095 !       1.56 eA-3
C195 0.405 0.667 0.854 !       1.56 eA-3
C196 0.469 0.978 0.514 !       1.54 eA-3
Q197 0.049 0.731 0.007 !       1.54 eA-3
C198 0.078 0.883 0.608 !       1.53 eA-3
C199 0.557 0.458 0.360 !       1.52 eA-3
;
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
Flack x determined using 2804 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         12141
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1390P)^2^+4.2594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2156
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.757
_reflns_Friedel_fraction_max     0.757
_reflns_number_gt                8445
_reflns_number_total             12141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04805f2.cif
_cod_data_source_block           CCDC_1475943
_cod_original_cell_volume        21252.3(5)
_cod_database_code               7124812
_cambridge_user_name             'Callum Benson'
_cambridge_user_crsid            cgmb3
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             CB152
_cambridge_data_id               dw_k3_0045
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              29448
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              78015