A Gel Aging Effect in the Synthesis of Open-Framework Gallium Phosphates: Structure Solution and Solid-State NMR of a Large-Pore, Open-Framework Material
Broom, Lucy; Clarkson, Guy J.; Guillou, Nathalie; Hooper, Joseph; Dawson, Daniel; Tang, Chiu; Ashbrook, Sharon Elizabeth; Walton, Richard I.; Dalton Transactions  (2017) –; doi:10.1039/C7DT03709K

data_7044781
_publ_section_title
;
 A Gel Aging Effect in the Synthesis of Open-Framework Gallium Phosphates:
 Structure Solution and Solid-State NMR of a Large-Pore, Open-Framework
 Material
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03709K
_journal_year                    2017
_chemical_formula_moiety         'F2.67 Ga7 O28 P6, 1.67(C4 H6 N2)'
_chemical_formula_sum            'C6.66 H9.99 F2.67 Ga7 N3.33 O28 P6'
_chemical_formula_weight         1309.30
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-03 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                104.626(5)
_cell_angle_beta                 100.346(5)
_cell_angle_gamma                101.936(4)
_cell_formula_units_Z            1
_cell_length_a                   5.0991(2)
_cell_length_b                   12.0631(6)
_cell_length_c                   13.8405(9)
_cell_measurement_reflns_used    4718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8860
_cell_measurement_theta_min      2.0790
_cell_volume                     781.41(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -107.00 22.00 1.00 80.00 -- -17.00 -72.00-180.00 129 2 \w -53.00 73.00 1.00 80.00 -- -17.00 0.00 150.00 126 3 \w -70.00 14.00 1.00 80.00 -- -17.00 -72.00 0.00 84 4 \w -35.00 69.00 1.00 80.00 -- -17.00 72.00 90.00 104 5 \w -30.00 -15.00 1.00 80.00 -- -17.00 -72.00 -90.00 15 6 \w -60.00 38.00 1.00 80.00 -- -17.00 0.00 -30.00 98'
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0676449000
_diffrn_orient_matrix_UB_12      0.0332331000
_diffrn_orient_matrix_UB_13      -0.0282579000
_diffrn_orient_matrix_UB_21      0.1275446000
_diffrn_orient_matrix_UB_22      -0.0090622000
_diffrn_orient_matrix_UB_23      0.0220648000
_diffrn_orient_matrix_UB_31      -0.0256961000
_diffrn_orient_matrix_UB_32      -0.0527728000
_diffrn_orient_matrix_UB_33      -0.0412171000
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9702
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.115
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku FRE+'
_exptl_absorpt_coefficient_mu    6.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_description       needle
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0502P)^2^+11.0678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2785
_reflns_number_total             3585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03709k2.cif
_cod_data_source_block           rw14newparts
_cod_database_code               7044781
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'O8 P2 Ga'
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.741
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O10, P2, O9, O11, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
3. Uiso/Uaniso restraints and constraints
C6 \\sim N4 \\sim C5 \\sim C3 \\sim N2 \\sim C1: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C4A \\sim C1A \\sim N2A \\sim C3A \\sim C6A \\sim N5A: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
O10 \\sim O9 \\sim P2 \\sim O8 \\sim O11: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 O11, O10, P2, O9, O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F3A)=Sof(Ga3A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(N2A)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(N5A)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(Ga3)=FVAR(1)
 Fixed Sof: N4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) N2(0.5) C3(0.5) H3(0.5)
 C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C3A(H3A), C4A(H4A), C6A(H6A)
6.b Fitted pentagon refined as free rotating group:
 N4(C5,C6,N2,C3), N2A(C3A,C4A,N5A,C6A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              25533
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
'Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling'
_oxdiff_exptl_absorpt_empirical_full_max 2.824
_oxdiff_exptl_absorpt_empirical_full_min 0.186