Multiple coordination modes of a new ditopic bis(pyrazolyl)methane-based ligand.
Coulton, John B.; Smith, Aramis C.; Wheeler, Kraig A.; Semeniuc, Radu F.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17109–17121; doi:10.1039/c8dt03992e

data_7048124
_publ_section_title
;
 Multiple coordination modes of a new ditopic bis(pyrazolyl)methane-based
 ligand.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17109
_journal_page_last               17121
_journal_paper_doi               10.1039/c8dt03992e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C16 H17 Ag N9 O), C F3 O3 S, C4 H10 O'
_chemical_formula_sum            'C37 H44 Ag2 B0 F3 N18 O6 S'
_chemical_formula_weight         1141.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.565(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2382(4)
_cell_length_b                   27.6761(10)
_cell_length_c                   7.7791(3)
_cell_measurement_reflns_used    3985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.03
_cell_measurement_theta_min      3.19
_cell_volume                     2415.10(15)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18285
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.211
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.493
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.5697
_exptl_crystal_description       plate
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.025
_platon_squeeze_details
;
Refinement with the un-SQUEEZED model resulted in a final R value of 6.03%.  
 Significant somewhat identifiable residual electron density was observed at
 the 3-4 e/A3 level suggesting the possible presence of disorded solvent
 (ether and/or acetone).  

 With space group Cm and Z=2, the 86 electrons correspond to 43 electrons 
 (86 electrons/2 = 43) in the asymmetric unit. Given electrons
 associated with acetonitrile (22) and ether (44), ether seems to
 be the match for the available electrons.  Since ether is the
 closest match in electron count, the formula should reflect the 
 inclusion of one molecule of ether per unit cell.
;
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1213 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4075
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.823
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                3427
_reflns_number_total             4075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03992e2.cif
_cod_data_source_block           15rfs09a_squeezed
_cod_depositor_comments
'Adding full bibliography for 7048124--7048128.cif.'
_cod_database_code               7048124
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.472
_shelx_estimated_absorpt_t_max   0.835
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              8225