Probing the Mechanistic and Energetic Basis for the Weak-Link Approach to Supramolecular Coordination Complexes
Holliday, Bradley J.; Jeon, You-Moon; Mirkin, Chad A.; Stern, Charlotte L.; Incarvito, Christopher D.; Zakharov, Lev N.; Sommer, Roger D.; Rheingold, Arnold L.; Organometallics 21 (2002) 5713–; doi:10.1021/om020739c

data_4077138
_publ_section_title
;
 Probing the Mechanistic and Energetic Basis for the Weak-Link Approach to
 Supramolecular Coordination Complexes
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5713
_journal_paper_doi               10.1021/om020739c
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety
'4(C76 H68 O4 P4 Rh2), 8(B F4), 3(C Cl2), C2 O'
_chemical_formula_sum            'C309 H272 B8 Cl6 F32 O17 P16 Rh8'
_chemical_formula_weight         6483.26
_chemical_name_systematic
; 
 [(m2,h1:h4:h1-(1,4-bis(2-(diphenylphosphino)ethoxy)naphthalene))2Rh2]
 [BF4]2 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.574(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   22.986(3)
_cell_length_b                   30.121(4)
_cell_length_c                   16.062(2)
_cell_measurement_temperature    153(2)
_cell_volume                     8571.9(19)
_computing_cell_refinement       'Bruker SAINT-1000 Diffractometer Control'
_computing_data_collection       'Bruker SMART-1000 Diffractometer Control'
_computing_data_reduction        'Bruker SAINT-1000 Diffractometer Control'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.484
_diffrn_measured_fraction_theta_max 0.484
_diffrn_measurement_device       'Bruker Smart 1000'
_diffrn_measurement_method       \w\
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25129
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.9058
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.631
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         10505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                9339
_reflns_number_total             10505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020739c.cif
_cod_data_source_block           complex8
_cod_depositor_comments
;
The following automatic conversions were performed:
'__computing_publication_material' tag replaced with
'_computing_publication_material'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8572(2)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4077138