Solid state coordination chemistry of oxomolybdenum‒organodiphosphonate materials: consequences of introducing xylyldiphosphonate components
Smith, Tiffany M.; Perkins, Kathryn; Symester, Diona; Freund, Steve R.; Vargas, Jose; Spinu, Leonard; Zubieta, Jon; CrystEngComm 16 (2014) 191–; doi:10.1039/c3ce41728j

data_7213580
_publ_section_title
;
 Solid state coordination chemistry of oxomolybdenum--organodiphosphonate
 materials: consequences of introducing xylyldiphosphonate components
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              191
_journal_paper_doi               10.1039/c3ce41728j
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C48 H40 Cu2 Mo5 N8 O21 P2, 6(H2 O)'
_chemical_formula_sum            'C48 H52 Cu2 Mo5 N8 O27 P2'
_chemical_formula_weight         1841.69
_chemical_name_systematic
;
 ?
;
_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-2013
_cell_angle_alpha                76.271(3)
_cell_angle_beta                 85.514(3)
_cell_angle_gamma                60.541(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0366(13)
_cell_length_b                   13.0703(13)
_cell_length_c                   20.989(2)
_cell_measurement_reflns_used    728
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.4666
_cell_measurement_theta_min      1.8989
_cell_volume                     3021.9(5)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33166
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.796
_exptl_absorpt_coefficient_mu    1.840
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_density_meas      2.05(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.063
_platon_squeeze_details
;
 The unit cell contains 3 water molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         2.145
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         10663
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8149
_reflns_number_total             10663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41728j.txt
_cod_data_source_block           mo_compound5
_cod_database_code               7213580
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2013-2