#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:42:55 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240881 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/04/4130457.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4130457
loop_
_publ_author_name
'Manna, Kuntal'
'Ji, Pengfei'
'Greene, Francis X.'
'Lin, Wenbin'
_publ_section_title
;
 Metal-Organic Framework Nodes Support Single-Site Magnesium-Alkyl
 Catalysts for Hydroboration and Hydroamination Reactions.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7488
_journal_page_last               7491
_journal_paper_doi               10.1021/jacs.6b03689
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '0(C312 H144 O64 Zr12)'
_chemical_formula_sum            'C0.99 H0.61 O0.2 Zr0.04'
_chemical_formula_weight         19.17
_chemical_name_systematic        TPHN-MgMe
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            632
_cell_length_a                   38.554(4)
_cell_length_b                   38.554(4)
_cell_length_c                   38.554(4)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100
_cell_measurement_theta_max      10.4215
_cell_measurement_theta_min      2.1936
_cell_volume                     57307(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.195
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'synchrotron, beamline 15-ID, APEX2 detector'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1248
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.195
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            193754
_diffrn_reflns_point_group_measured_fraction_full 0.195
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         14.560
_diffrn_reflns_theta_min         0.869
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.351
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             6112
_refine_diff_density_max         0.446
_refine_diff_density_min         -2.153
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.1132
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3252
_refine_ls_wR_factor_ref         0.3402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1761
_reflns_number_total             2572
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b03689_si_002.cif
_cod_data_source_block           mg0519-1_a
_cod_original_cell_volume        57306(19)
_cod_original_formula_sum        'C0.99 H0.61 O0.20 Zr0.04'
_cod_database_code               4130457
_shelxl_version_number           2013-4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-C2
 1.54 with sigma of 0.02
 C2-C3
 1.4 with sigma of 0.02
 C3-C4
 1.4 with sigma of 0.02
 C4-C5
 1.4 with sigma of 0.02
 C5-C6
 1.54 with sigma of 0.02
 C2-C4
 2.425 with sigma of 0.02
 C3-C5
 2.425 with sigma of 0.02
 C2-C5
 2.75 with sigma of 0.02
 C6-C7
 1.4 with sigma of 0.02
 C7-C8
 1.4 with sigma of 0.02
 C6-C8
 2.425 with sigma of 0.02
 C9-C8
 1.4 with sigma of 0.02
 C9-C7
 2.425 with sigma of 0.02
 C5-C7
 2.547 with sigma of 0.02
 C6-C9
 2.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7)
;
