Extracting structural trends from systematic variation of phosphonate/phosphonate monoester coordination polymers
Gelfand, Benjamin S.; Taylor, Jared M.; Shimizu, George K. H.; CrystEngComm  (2017) –; doi:10.1039/C7CE00579B

data_7228449
_publ_section_title
;
 Extracting structural trends from systematic variation of
 phosphonate/phosphonate monoester coordination polymers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00579B
_journal_year                    2017
_chemical_formula_moiety         'C30 H70 Ba3 O29 P6, H2 O'
_chemical_formula_sum            'C30 H72 Ba3 O30 P6'
_chemical_formula_weight         1510.69
_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_date             2017-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                67.65(3)
_cell_angle_beta                 82.28(3)
_cell_angle_gamma                82.80(3)
_cell_formula_units_Z            2
_cell_length_a                   11.616(2)
_cell_length_b                   15.242(3)
_cell_length_c                   17.613(4)
_cell_measurement_reflns_used    842
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2848.6(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23197
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.732
_diffrn_reflns_theta_min         1.775
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M., SADABS 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         12932
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0614
_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^)+35.9180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10159
_reflns_number_total             13391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00579b1.cif
_cod_data_source_block           4
_cod_database_code               7228449
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O19(H19A,H19B), O20(H20A,H20B), O21(H21A,H21B), O22(H22A,H22B), O23(H23D,
 H23E), O24(H24D,H24E), O25A(H25A,H25B), O26(H26D,H26E), O27(H27D,H27E),
 O28(H28A,H28B), O30(H30D,H30E), O29(H29D,H29E)
3.b Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C22(H22), C25(H25), C28(H28)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C17(H17), C19(H19), C21(H21)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              55885
_olex2_submission_special_instructions 'No special instructions were received'