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_7048128
_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_sum            'C22 H17 Br2 N9 O7 Re2'
_chemical_formula_weight         1051.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                63.050(2)
_cell_angle_beta                 78.311(2)
_cell_angle_gamma                71.078(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4206(4)
_cell_length_b                   13.4302(5)
_cell_length_c                   13.6824(6)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.18
_cell_measurement_theta_min      3.63
_cell_volume                     1611.15(12)
_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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.977
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36153
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.632
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.835
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.058
_platon_squeeze_details
;
Refinement with the un-SQUEEZED model resulted in a final R value of 3.06%.  
 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 P-1 and Z=2, the 49 electrons correspond to 24.5 electrons 
 (49 electrons/2 = 24.5) in the asymmetric unit. Given electrons
 associated with acetone (32) and ether (42), neither solvent is
 an ideal match for the available electrons.  Since ether is 
 closest in electron count, the formula should reflect the 
 incllusion of one molecule of ether per unit cell.
;
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5772
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0245P)^2^+3.8040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5643
_reflns_number_total             5772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03992e2.cif
_cod_data_source_block           16rfs03_sq_sqd
_cod_depositor_comments
'Adding full bibliography for 7048124--7048128.cif.'
_cod_original_cell_volume        1611.16(12)
_cod_database_code               7048128
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.135
_shelx_estimated_absorpt_t_max   0.424
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              16785